Method of treating depression with arylglycinamide derivatives
Granted 2 Jul 2002 · no office action yet
Current assignee: Boehringer Ingelheim Kg · originally Boehringer Ingelheim International GmbH
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Inventors: Hans Briem, Gerd Schnorrenberg, Franz Esser, Horst Dollinger +2 · Examiner: Robert W. Ramsuer · AU 1626 · TC 1600
Life of the application
4 dated eventsAbstract
The invention relates to new arylglycinamide derivatives of general formula I and the pharmaceutically acceptable salts thereof, wherein R1 and R2 together with the N to which they are bound form a ring of the formula whereinp is 2 or 3 andX denotes oxygen, N(CH2)nR6 or CR7R8,and R3, R4, R5, R6, R7, R8, Ar and n have the meanings given in the specification, and the preparation and use thereof. The new compounds are valuable neurokinin (tachykinin)-antagonists.
Description
84 parts›CROSS REFERENCE TO RELATED APPLICATIONS
This application is a division of application Ser. No. 09/752,730, filed Jan. 3, 2001, now U.S. Pat. No. 6,303,601, which is a division of application Ser. No. 09/507,581, filed Feb. 18, 2000, now U.S. Pat. No. 6,251,909, which is a division of application Ser. No. 08/930,704, §102(e) date Oct. 29, 1997, now U.S. Pat. No. 6,124,296, which is the National Stage of International Application No. PCT/EP96/01548, filed Apr. 11, 1996.
›SUMMARY OF THE INVENTION
The invention relates to new arylglycinamide derivatives of general formula I
and the pharmaceutically acceptable salts thereof, processes for preparing them and pharmaceutical compositions containing these compounds. The compounds are valuable neurokinin (tachykinin) antagonists.
›DETAILED DESCRIPTION OF THE INVENTION · 1 of 3
The abbreviations used in the specification and claims are explained as follows:
CDI=Carbonyldiimidazole
DCCI=Dicyclohexylcarbodiimide
HOBt=1-Hydroxybenzotriazole
THF=Tetrahydrofuran
DMF=Dimethylformamide
RT=Room temperature
DMAP=4-Dimethylaminopyridine
TBTU=O-Benzotriazolyl-tetramethyluroniumtetrafluoroborate
In order to show the formulae, a simplified representation is used. In the representation of the compounds all CH 3 -substituents are represented by a single bond, and for example the following formula
represents
The invention relates to new aryiglycinamide derivatives of general formula I
or the pharmaceutically acceptable salts thereof,
wherein
Ar denotes unsubstituted or mono- to pentasubstituted phenyl, or unsubstituted or mono- or di-substituted naphthyl, [in which the substituents of the phenyl and naphthyl independently of each other denote halogen (F, Cl, Br, I), OH, (C 1-4 )alkyl, O—(C 1-4 )alkyl, CF 3 , OCF 3 or NR 9 R 10 (wherein R 9 and R 10 independently of each other denote H, methyl or acetyl)] or Ar is phenyl'substituted by —OCH 2 O— or —O(CH 2 ) 2 O—;
R 1 and R 2 together with the N to which they are bound form a ring of the formula
wherein
p is 2 or 3,
X denotes oxygen, N(CH 2 ) n R 6 or CR 7 R 8 , wherein
n is 0, 1 or 2,
R 6 is (C 3-7 )cycloalkyl, phenyl or naphthyl, wherein the phenyl may be mono- to tri-substituted by halogen (F, Cl, Br, I), (C 1-4 )alkyl, O—(C 1-4 )alkyl, CF 3 , OCF 2 or NR 15 R 16 (wherein R 15 and R 16 independently of each other denote H, methyl or acetyl);
R 7 and R 8 have one of the following meanings:
a) R 7 and R 8 represent H if R 3 is unsubstituted or substituted phenyl,
b) R 7 is phenyl, phenyl substituted by 1 to 3 substituents [wherein the substituents independently of one another denote halogen (F, Cl, Br, I), (C 1-4 )alkyl, O—(C 1-4 )alkyl, CF 3 or OCF 3 ], piperidinyl, 1-methylpiperidinyl,
if R 8 is H, —CONH 2 , —NHC(O)CH 3 , —N(CH 3 )C(O)CH 3 , CN
or —C(O)N((C 1-3 )alkyl) 2 or
c) R 7 and R 8 together form the group
R 3 denotes H, (C 1-4 )alkyl, unsubstituted or mono- to tri-substituted phenyl, wherein the substituents independently of one another represent halogen (F, Cl, Br, I), (C 1-4 )alkyl, O—(C 1-4 )alkyl, CF 3 , OCF 3 or NR 17 R 18 (wherein R 17 and R 18 independently of one another denote H, methyl or acetyl);
R 4 denotes phenyl(C 1-4 )alkyl or naphthyl(C 1-4 )alkyl, wherein phenyl may be substituted by 1 to 3 substituents, wherein the substituents independently of one another are halogen (F, Cl, Br, I), (C 1-4 )alkyl, O—(C 1-4 )alkyl, CF 3 , OCF 3 or NR 19 R 20 (wherein R 19 and R 20 independently of one another denote H, methyl or acetyl); and
R 5 denotes H, (C 1-4 )alkyl, (C 3-6 )cycloalkyl, CH 2 COOH, —CH 2 C(O)NH 2 , —OH or phenyl(C 1-4 )alkyl.
The compounds according to the invention are valuable neurokinin (tachykinin) antagonists which have both substance P-antagonism and also neurokinin A- or neurokinin B-antagonistic properties. They are useful for the treatment and prevention of neurokinin-mediated diseases.
Compounds of general formula I may contain acid groups, chiefly carboxyl groups, and/or basic groups such as, for example, amino functions. Compounds of general formula I may therefore be obtained either as internal salts, as salts with pharmaceutically acceptable inorganic acids such as hydrochloric acid, sulphuric acid, phosphoric acid or sulphonic acid or organic acids (such as, for example, maleic acid, fumaric acid, citric acid, tartaric acid or acetic acid) or as salts with pharmaceutically acceptable bases such as alkali or alkaline earth metal hydroxides or carbonates, zinc or ammonium hydroxides or organic amines such as, for example, diethylamine, triethylamine or triethanolamine, etc.
The compounds according to. the invention may occur as racemates but may also be obtained as pure enantiomers, i.e. in (R)- or (S)-form. They may also occur as diastereoisomers or mixtures thereof.
The preferred compounds of general formula I are those wherein
R 1 and R 2 together with the N to which they are bound form a 6-membered ring of the formula
wherein
X denotes N(CH 2 ) n R 6 or CR 7 R 8 ,
wherein n, R 6 , R 7 and R 8 are defined as in claim 1 .
Particular mention should be made of compounds of formula I wherein
X is N(CH 2 ) n R 6 wherein n is 0, 1 or 2 and R 6 is (C 3-7 )cycloalkyl or phenyl, particularly those compounds wherein n is 0 and R 6 is (C 3-7 )cycloalkyl, particularly those compounds wherein R 6 is cyclobutyl or cyclohexyl.
Mention should also be made of compounds of formula I wherein
R 7 and R 8 have one of the following meanings:
a) R 7 and R 8 denote H when R 3 is unsubstituted or substituted phenyl,
b) R 7 is phenyl, piperidinyl
if R 8 is H, —CONH 2 , —NHC(O)CH 3 , —N(CH 3 )C(O)CH 3 or CN, or
c) R 7 and R 8 together form the group
particularly those wherein
R 7 and R 8 have one of the following meanings:
a) R 7 and R 8 denote H when R 3 is unsubstituted or substituted phenyl,
b) R 7 is phenyl,
when R 8 is H, —CONH 2 or CN, or
c) R 7 and R 8 together form the group
The preferred compounds are those wherein
R 7 denotes phenyl
and R 8 is H or CN, particularly those wherein R 7 is pyridino and R 8 is H.
Of the compounds defined above, the preferred ones are those wherein
Ar denotes unsubstituted or mono- or di-substituted phenyl, or unsubstituted naphthyl [wherein the substituents of the phenyl independently of one another are halogen (F, Cl, Br, I), OH, methyl, methoxy, CF 3 , OCF 3 or dimethylamine] or Ar is phenyl substituted by —OCH 2 O—, this group connecting positions 2 and 3 or 3 and 4 of the phenyl, particularly those wherein
Ar denotes unsubstituted or mono- or di-substituted phenyl, or unsubstituted naphthyl [wherein the substituents of the phenyl independently of one another are halogen (F, Cl, Br), methoxy or CF 3 ] or Ar is phenyl substituted by —OCH 2 O—, this group connecting positions 2 and 3 or 3 and 4 of the phenyl.
The preferred compounds are those wherein Ar is phenyl, 3,4-dichlorophenyl, 3,4-dimethoxyphenyl or 3,4-methylenedioxyphenyl.
›DETAILED DESCRIPTION OF THE INVENTION · 2 of 3
Of the compounds defined above, particular mention should be made of those wherein R 3 is phenyl or preferably H.
Of the compounds defined above, mention should also be made of those wherein
R 4 denotes phenyl(C 1-3 )alkyl, wherein phenyl may be substituted by 1 or 2 substituents, the substituents independently of one another being halogen (F, Cl, Br, I), methyl, methoxy, CF 3 or OCF 3 ; and
R 5 denotes H, (C 1-3 )alkyl, CH 2 COOH, —CH 2 C(O)NH 2 or phenethyl,
particularly those compounds wherein
R 4 is
and R 5 denotes H or CH 3 .
The following compounds are preferred:
The term naphthyl used above includes both 1-naphthyl and 2-naphthyl.
Test results for compounds according to the invention:
The receptor affinity for the NK 1 -receptor (substance P-receptor) is determined on human lymphoblastoma cells (IM-9) with cloned NK 1 -receptors, measuring the displacement of 125 I-labelled substance P. The K i -values thus obtained demonstrate the efficacy of the compounds:
The compounds according to the invention are valuable neurokinin (tachykinin) antagonists which have, in particular, NK 1 -antagonism, but also NK 2 - and NK 3 -antagonistic properties.
The compounds according to the invention are valuable neurokinin (tachykinin) antagonists which have both substance P-antagonism and also neurokinin A- or neurokinin B-antagonistic properties. They are useful for the treatment and prevention of neurokinin-mediated diseases: treatment and prevention of inflammatory and allergic diseases of the respiratory tract, such as asthma, chronic bronchitis, emphysema, rhinitis or coughs, eye diseases such as conjunctivitis and iritis, skin diseases such as dermatitis in contact eczema, urticaria, psoriasis, sunburn, insect bites and stings, neurodermitis, itching and postherpetic pain,
diseases of the gastrointestinal tract such as gastric and duodenal ulcers, ulcerative colitis, Crohn's disease, irritable bowel, Hirschsprung's disease;
diseases of the joints such as rheumatoid arthritis, reactive arthritis and Reiter'syndrome;
for treating diseases of the central nervous system such as dementia, Alzheimer's disease, schizophrenia, psychosis, depression, headaches (e.g. migraine or tension headaches) and epilepsy;
for the treatment of tumours, collagenosis, dysfunction of the urinary tract, haemorrhoids, nausea and vomiting, triggered for example by radiation or cytostatic therapy or motion and pain of all kinds.
The invention therefore also relates to the use of the compounds according to the invention as remedies and pharmaceutical preparations which contain these compounds. They are preferably for use in humans. The compounds according to the invention may be administered by intravenous, subcutaneous, intramuscular, intraperitoneal or intranasal route or by inhalation, by transdermal route, if desired with the aid of iontophoresis or enhancers known from the literature, and by oral route.
For parenteral administration, the compounds of formula I or the physiologically acceptable salts thereof, optionally with conventional substances such as solubilisers, emulsifiers or other adjuvants, may be made into solutions, suspensions or emulsions. Suitable solvents include, for example, water, physiological saline solutions or alcohols, e.g. ethanol, propanediol or glycerol, sugar solutions such as glucose or mannitol solutions or a mixture of various solvents.
In addition, the compounds may be administered by means of implants, e.g. of polylactide, polyglycolide or polyhydroxybutyric acid or by means of intranasal preparations.
The oral effectiveness of compounds of general formula I can be demonstrated using the following standard test:
Inhibition of the lowering of blood pressure caused by NK 1 in anaesthetised guinea pigs.
Guinea pigs weighing 300-500 grams were anaesthetised with pentobarbital (50 mg/kg i.p.), intubated and mechanically ventilated with 10 ml of ambient air per kg of body weight at a rate of 60 breaths per minute. The blood pressure was measured in the blood flow through the carotid artery. In order to introduce substances intravenously, the jugular vein was cannulated.
By the intravenous administration of the NK 1 -agonist [βAla 4 , Sar 9 , Met(O 2 ) 11 ] SP(4-11) (0.2 μmol/kg) a brief lowering of the blood pressure was triggered which was repeated at 10 minute intervals by repeatedly giving the NK 1 -agonist.
The neurokinin-antagonist was then administered by intraduodenal route and at 10 minute intervals a lowering of blood pressure was induced by means of the NK 1 -agonist.
The inhibition of the lowering of blood pressure caused by the above-mentioned NK 1 -agonist was measured before and after treatment with the neurokinin-antagonist.
The compound of Example 5 yielded an ID 50 of 1.4 mg/kg. (ID 50 is the dose which inhibits the lowering of blood pressure caused by the NK 1 -agonist by 50%.)
The compounds according to the invention may be prepared by generally known methods.
The compounds may be prepared in various ways. The two commonest methods are shown in the following scheme:
Method A. The carboxylic acid may be linked to the amine HN(R 5 )R 4 in various ways. The usual methods are coupling methods such as those used in peptide chemistry. A coupling reagent such as TBTU, DCCI/HOBt, CDI, etc., is added to the coupling partners in an approximately equivalent amount. Suitable solvents are DMF, THF, CH 2 Cl 2 , CHCl 3 , acetonitrile or other inert solvents or mixtures thereof. The appropriate temperature range is between −50° C. and +120° C., preferably between 0° C. and 40° C.
The carboxylic acid may also initially be converted by means of SOCl 2 , SO 2 Cl 2 , PCl 3 , PCl 5 or PBr 3 or mixtures thereof, by known methods, into the corresponding acid halide which is subsequently reacted with the amine HN(R 5 )R 4 in an inert solvent such as CH 2 Cl 2 , THF or dioxane at temperatures between −50° C. and +100° C., typically between 0° C. and 20° C.
Another alternative is to convert the carboxylic acid initially into the alkylester, usually the methylester, by known methods and then to react this ester with the amine HN(R 5 )R 4 in an inert solvent such as DMF, dioxane or THF. The reaction temperatures are between 20° C. and 150° C., typically between 50° C. and 120° C. The reaction may also be carried out in a pressurised container.
›DETAILED DESCRIPTION OF THE INVENTION · 3 of 3
Process B. In this, the α-halo-arylacetamide derivative obtained according to known procedures is reacted with the amine R 1 (R 2 )NH, thereby generating hydrogen halide. In order to mop up the cleaved (or excess) hydrogen halide, inorganic bases are used such as K 2 CO 3 , NaHCO 3 or CaCO 3 , or organic bases may be used such as triethylamine, Hung base, pyridine or DMAP, or an excess of the amine R 1 (R 2 )NH may be used. DMF, THF, dioxane or other inert solvents are used. The temperature range for the reaction is from 0 to 100° C., typically from 10 to 80° C.
Process C. The compounds according to the invention in which R 5 is not H may also be prepared as follows: first of all, the corresponding compound in which R 5 is H is synthesised according to process A or B. Then N-alkylation is carried out as follows in order to introduce alkyl, cycloalkyl or CH 2 COOH. The compound according to the invention wherein R 5 is H is deprotonated with an equivalent quantity of NaH, NaNH 2 , KOH, NaOCH 3 or some other strong base. Anhydrous inert solvents such as THF, dioxane or diethylether are used. Then the corresponding alkylating agent is added slowly in the form of the corresponding halide, tosylate or mesylate. The reaction is carried out in the temperature range from −50° C. to +100° C., typically between 0° C. and +50° C. The method is described in detail in Example 33.
›Examples79
›EXAMPLE 1
1st Step: 2.2 g of 1-cyclohexylpiperazine were dissolved in 150 ml of anhydrous DMF, mixed with 2 g of K 2 CO 3 , stirred at room temperature for 20 minutes and then cooled to 5° C. 2.7 g of methyl (R,S)-α-bromophenylacetic acid were added and the suspension was stirred overnight at RT. The precipitate was filtered off and the filtrate was evaporated down. The residue was taken up in ethyl acetate, extracted twice with 10%. KHCO 3 solution and once with saturated NaCl solution. The organic phase was dried over Na 2 SO 4 , filtered and evaporated down, and 3.7 g of (R,S)-1-cyclohexyl-4-(methyl 2-phenylacetate)piperazine were obtained in the form of a yellow oil. Yield: about 100%.
2nd Step: 2.3 g of the product of the first step were dissolved in 10 ml of methanol, mixed with 14 ml of 1N NaOH and the resulting emulsion was stirred overnight at room temperature. The clear reaction solution was neutralised by the addition of 14 ml of 1N HCl, evaporated to dryness, the residue was treated with isopropanol and the solid matter was collected by suction filtration. The filtrate was evaporated down and the residue was triturated again with isopropanol, the solid matter was suction filtered and combined with the solid obtained earlier. In this way, 1.6 g of (R,S)-1-cyclohexyl-4-(2-phenylacetic acid) -piperazine were obtained as a white solid.
Yield: 75%.
3rd Step: 0.6 g of the product of the second step, 0.48 g of 3,5-bis-(trifluoromethyl)-benzylamine and 0.32 g of HOBT were suspended in 60 ml of THF/CH 2 Cl 2 (1:1) and adjusted to pH 8.5 by the addition of about 0.7 ml of Hünig base. 0.77 g of TBTU were added and the mixture was stirred overnight at room temperature. The clear reaction solution was evaporated down in vacuo, the residue was taken up in CH 2 Cl 2 and extracted twice with 10% KHSO 4 solution, once with saturated NaCl solution, twice with 10% KHCO 3 solution and once more with saturated NaCl solution. The organic phase was dried over Na 2 SO 4 , filtered and evaporated down, whereupon crystallisation took place. 0.685 g of (R,S)-1-cyclohexyl-piperazinyl-4-[2-phenylacetic acid-N-(3,5-bis-trifluoromethylbenzyl)amide] were obtained as a yellowish solid. Yield 64%.
Mp: 124-129° C. FAB-MS: (M+H) + =528.2.
›EXAMPLE 2
1st Step: 0.49 g of 3,5-bis-(trifluoromethyl)-benzylamine were dissolved in 30 ml of anhydrous CH 2 Cl 2 , 0.3 ml of triethylamine were added, the mixture was cooled in an ice bath and over 20 minutes a solution of 0.46 g of (R,S)-α-bromophenylacetyl chloride in 10 ml of CH 2 Cl 2 was added dropwise. After the mixture had stood at room temperature over a weekend, the solvent was eliminated and the solid residue was triturated with diethylether, suction filtered and the filtrate was evaporated down. 0.6 g of α-bromophenylacetic acid N-(bis-trifluoromethylbenzyl)-amide were obtained as a light beige solid.
Yield: 43.5%.
2nd Step: 0.21 g of 4-propionylamino-piperidine hydrochloride were dissolved in 30 ml of anhydrous DMF, 0.33 g of K 2 CO 3 were added and the mixture was stirred for 30 minutes at room temperature. Over 20 minutes a solution of 0.68 g of the product of the first step in 10 ml of DMF were added dropwise to this mixture, which was then stirred overnight at room temperature. The suspension was filtered, the filtrate was evaporated down, the oily residue obtained was taken up in ethyl acetate, extracted twice with 10% KHCO 3 solution and once with saturated NaCl solution. The organic phase was dried over Na 2 SO 4 , filtered, the filtrate was evaporated down and the semi-solid residue obtained was triturated with diethylether and suction filtered. 0.33 g of (R,S)-4-propionylamino-1-[2-phenylacetic acid-N(3,5-bis-trifluoromethyl-benzyl)-amide]-piperidine were obtained as a white solid.
Yield: 64%. Mp: 189-191° C. FAB-MS: (M+H) + =516.4.
›EXAMPLE 33
Mp: >240° C.; FAB-MS: (M+H) + =556.4
0.3 g of the compound according to Example 25 were converted into the corresponding base by treatment with KHCO 3 and dried. The resulting product was dissolved in 5 ml of anhydrous THF, 34 mg of NaH (60% in oil) were added and the mixture was stirred for 1.5 hours at room temperature. Then 0.1 g of methyliodide were added and the mixture was stirred overnight. The reaction mixture was mixed with 2 ml of THF/water (1:1) then with 25 ml of water and extracted 3 times with ether. The combined ether extracts were dried over Na 2 SO 4 and evaporated down in vacuo, thereby obtained 170 mg of the desired compound in the form of a free base (oil). This was converted into the dihydrochloride by the addition of an excess of ethereal HCl, the dihydrochloride being obtained in the form of yellow crystals.
Yield: 113 mg (36%).
The other compounds of the invention may be prepared analogously, e.g. as follows:
›EXAMPLE 3
Mp 235-238° C. FAB-MS: (M+H) + =542.2.
›EXAMPLE 4
Mp: >240° C. (Decomp.). FAB-MS: (M+H) + =542.3.
›EXAMPLE 5
Mp: 158-164° C.; FAB-MS: (M+H) + =556.4.
›EXAMPLE 6
Mp: 97-99° C.; FAB-MS: (M+H) + =556.3.
›EXAMPLE 7
Mp: >240° (Decomp.); FAB-MS: (M+H) + =528.4.
›EXAMPLE 8
Mp: 102-105° C.; FAB-MS: (M+H) + =640.3.
›EXAMPLE 9
Mp: 141-149° C.; FAB-MS: (M+H) + =579.2.
›EXAMPLE 10
Mp: 218-223° C.; FAB-MS: (M+H) + =579.3.
›EXAMPLE 11
Mp: >220° (Decomp.); FAB-MS (M+H) + =571.3
›EXAMPLE 12
Mp: 205-210° C.; FAB-MS: (M+H) + =591.3.
›EXAMPLE 13
Mp: 87-95° C.; FAB-MS: (M+H) + =571.2
›EXAMPLE 14
Mp: 164-166° C.; FAB-MS: (M+H) + =537.3.
›EXAMPLE 15
Mp: 208-210° C.; FAB-MS: (M+H) + =578.3.
›EXAMPLE 16
Mp: 110-115° C.; FAB-MS: (M+H) + =542.3.
›EXAMPLE 17
Mp: 118-123° C.; FAB-MS: (M+H) + =556.3
›EXAMPLE 18
Mp: 134-136° C.; FAB-MS: (M+H) + =514.3
›EXAMPLE 19
Mp: >240° (Decomp.): FAB-MS: (M+H) + =564
›EXAMPLE 20
Mp: 180-185° C.; FAB-MS: (M+H) + =564.3
›EXAMPLE 21
Mp: 228-232° C.; FAB-MS: (M+H) + =606/608
›EXAMPLE 22
Mp: 70-73° C.; FAB-MS: (M+H) + =586
›EXAMPLE 23
Mp: 248-254° C.; FAB-MS: (M+H) + =596/598/600
›EXAMPLE 24
Mp: 210° C.; FAB-MS: (M+H) + =664.1
›EXAMPLE 25
Mp: 192-199° C.; FAB-MS: (M+H) + =542.3
›EXAMPLE 26
Mp: 112-118° C.; FAB-MS: (+H) + =562/564
›EXAMPLE 27
Mp: 124-127° C.; FAB-MS: (M+H) + =606/608
›EXAMPLE 28
Mp: 118-120° C.; FAB-MS: (M+H) + =606/608
›EXAMPLE 29
Mp: 120-122° C.; FAB-MS: (M+H) + =562/564
›EXAMPLE 30
Mp: >240° C.; FAB-MS: (M+H) + =562/564
›EXAMPLE 31
Mp: >240° C.; FAB-MS: (M+H) + =546.3
›EXAMPLE 32
Mp: 125-130° C. (Decomp); FAB-MS: (M+H) + =610.4
›EXAMPLE 33
Mp: >240° C.; FAB-MS: (M+H) + =556.4
›EXAMPLE 34
Mp: 145-151° C.; FAB-MS: (M+H) + =641.3
›EXAMPLE 36
Mp: 175-176.5° C.
›EXAMPLE 37
Mp: 157-158° C.
›EXAMPLE 38
Mp: 155-172° C. FAB-MS: (M+H) + =592.2
›EXAMPLE 42
Mp: 142-150° C. FAB-MS: (M+H) + =558.2
›EXAMPLE 44
Mp: 107-111° C.; FAB-MS: (M+H) + =575.6
›EXAMPLE 45
M.p: >230° C.
›EXAMPLE 46
M.p: >230° C.
›EXAMPLE 47
M.p: 127-137° C. FAB-MS: (M+H) + =592
›EXAMPLE 50
M.p. 106-110° C. FAB-MS: (M+H) + =549.4
›EXAMPLE 52
Mp: 133-143° C. FAB-MS: (M+H) + =542.3
›EXAMPLE 53
M.p. 110-120° C. FAB-MS: (M+H) + =570.4
›EXAMPLE 58
Mp: 212-216° C. (Decomp.) FAB-MS: (M+H) + =624.3/626.3/628.3
›EXAMPLE 59
Mp: 244-246° C. (Decomp.) FAB-MS: (M+H) + =624.1/626.2/628
›EXAMPLE 60
Mp: 113-123° C. FAB-MS: (M+H) + =550.3
›EXAMPLE 61
Mp: 195-205° C.
›EXAMPLE 62
Mp: 210-218° C. FAB-MS: (M+H) + =620/622
›EXAMPLE 63
Mp: 215-224° C. FAB-MS: (M+H) + =576/578
›EXAMPLE 64
Mp: 85-92° C. FAB-MS: (M+H) + =572.5
›EXAMPLE 65
Mp: 148-156° C. FAB-MS: (M+H) + =578.4
›EXAMPLE 66
Mp: 113-117° C. (decomp.) FAB-MS: (M+H) + =528.5
›EXAMPLE 67
Mp: 265-268° C. (decomp.) FAB-MS: (M+H) + =619.3
›EXAMPLE 68
Mp: 236-238° C. (decomp.) FAB-MS: (M+H) + =528.3
›EXAMPLE 69
Mp: 177-187° C. FAR-MS: (M+H) + =605.3
›EXAMPLE 70
Mp: 123-133° C. (decomp.) FAB-MS: (M+H) + =616.3
›EXAMPLE 71
Mp: 87-97° C. FAB-MS: (M+H) 30 =600.2
›EXAMPLE 72
Mp: >230° C.
›EXAMPLE 73
Mp: >230° C.
›EXAMPLE 74
Mp: >230° C.
›EXAMPLE 75
Mp: 91-98° C. FAB-MS: (M+H) + =574.4
›EXAMPLE 76
Mp: 234-236° C.
›EXAMPLE 77
Mp: 195-198° C.
›EXAMPLE 78
Pharamaceutical Preparations
sufficient water to make a 10 ml solution for injection
sufficient water to make a 10 ml solution for injections
Dosage for humans weighing 67 kg: 1 to 500 mg
›Tables in the description — 3
| Compound of Example 3: | 1.4 nM |
| Compound of Example 4: | 1.0 nM |
| Cornpound of Example 5: | 1.3 nM |
| Compound of Example 33: | 1.3 nM |
| Compound of Example 45: | 1.6 nM |
| Compound of Example 46: | 1.4 nM |
| Compound of Example 52: | 1.1 nM |
| Compound of Example 53: | 2.3 nM |
| Compound of Example 58: | 6.4 nM |
| Compound of Example 59: | 4.2 nM |
| Compound of Example 65: | 9.2 nM |
| Compound of Example 66: | 1.4 nM |
| Compound of Example 68: | 1.5 nM |
| Compound of Example 70: | 2.8 nM |
| Compound of Example 71: | 2.1 nM |
| Compound of Example 72: | 6.8 nM |
| Compound of Example 73: | 1.7 nM |
| Compound of Example 74: | 11.8 nM |
| Compound of Example 75: | 180 nM |
| Compound of Example 76: | 7.0 nM |
| 200 mg | of active substance* | |
| 1.2 mg | of monopotassium dihydrogen phospate = KH 2 PO 4 | ) |
| 0.2 mg | of disodium hydrogen phosphate = | ) (buffer) |
| NaH 2 PO 4 .2H 2 O | ) | |
| 94 mg | of sodium chloride | ) |
| or | ) (isotonic) | |
| 520 mg | of glucose | ) |
| 4 mg | of albumin | (protease protection) |
| q.s. | sodium hydroxide solution | ) |
| q.s. | hydrochloric acid | ) to adjust the pH |
| to pH 6 |
| 200 mg | of active substance* | |
| 94 mg | of sodium chloride | |
| or | ||
| 520 mg | of glucose | |
| 4 mg | of albumin | |
| q.s. | sodium hydroxide solution | ) |
| q.s. | hydrochloric acid | ) to adjust the pH |
| to pH 9 |
Claims as granted
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21 codes- A61P25/24
- C07D295/145
- C07D211/64
- C07D211/66
- C07D211/62
- C07D211/58
- C07D401/12
- C07D471/10
- C07D401/04
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