IP Library Patent Application 14661063
Patent Application
App. No. 14/661,063

TETRAHYDROISOQUINOLINES AND INTERMEDIATES THEREFOR

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Patent No.
US None
App. No.
14/661,063
Abstract

Disclosed are processes for preparing tetrahydroisoquinolines, intermediates useful in the preparation of tetrahydroisoquinolines, processes for preparing such intermediates, and a crystalline form of 6-[(4S)-2-methyl-4-(naphthyl)-1,2,3,4-tetrahydroisoquinolin-7-yl]pyridazin-3-amine. Also disclosed are pharmaceutical compositions comprising tetrahydroisoquinolines, methods of using tetrahydroisoquinolines in the treatment of depression and other conditions and methods for obtaining the crystalline form.

Claims (78)

1 . A compound having the following formula:

where R 1 is selected from the group consisting of Br and H 3 CO.

2 . A compound of claim 1 having the following formula:

3 . A compound having the following formula:

where R 1 is selected from the group consisting of Br and H 3 CO.

4 . A compound of claim 3 having the following formula:

5 . A compound having the following formula:

where R 2 is selected from the group consisting of Br, H 3 CO and HO.

6 . A compound of claim 5 having the following formula:

7 . A compound having the following formula:

where R 3 is selected from the group consisting of

where R 4 is C 1 -C 4 alky, aryl or phenyl, and n is 1 or 2.

8 . A compound of claim 7 having the following formula

9 . A compound having the following formula:

Where each R 5 is independently selected from the group consisting of hydrogen t-butoxycarbonyl, carboxybenzyl, para-methoxybenzylcarbonyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, benzyl, 9-fluorenylmethyloxycarbonyl, N-phthalimide, COCH 3 and COCF 3 .

10 . A compound of claim 9 having the following formula:

11 . A compound having the following formula:

Where each R 5 is selected from the group consisting of hydrogen, t-butoxycarbonyl, carboxybenzyl, para-methoxybenzylcarbonyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, benzyl, 9-fluorenylmethyloxycarbonyl, N-phthalimide, COCH 3 and COCF 3 .

12 . A compound of claim 11 having the following formula:

13 . A compound having the following formula:

where each R 5 is selected from the group consisting of hydrogen, t-butoxycarbonyl, carboxybenzyl, para-methoxybenzylcarbonyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, benzyl, 9-fluorenylmethyloxycarbonyl, N-phthalimide, COCH 3 and COCF 3 .

14 . A compound of claim 13 having the following formula:

15 . A compound having the following formula:

Where each R 5 is selected from the group consisting of hydrogen, t-butoxycarbonyl, carboxybenzyl, para-methoxybenzylcarbonyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, benzyl, 9-fluorenylmethyloxycarbonyl, N-phthalimide, COCH 3 and COCF 3 , and X is selected from the group consisting of Cl, Br, I and trifluoromethanesulfonyloxy.

16 . A compound of claim 15 having the following formula:

17 . A process of making a compound having the formula:

where R 2 is selected from the group consisting of Br, H 3 CO and HO, comprising reacting a compound having the formula:

where R 1 is selected from Br or H 3 CO, under conditions effective to promote the formation of Compound 17R.

18 . A process of making a compound having the formula:

comprising reacting a compound having the formula:

under conditions effective to promote the formation of compound 6.

19 . A process of making a compound having the formula:

comprising reacting a compound having the formula;

where R 2 is selected from the group consisting of Br, H 3 CO and HO,

under conditions effective to promote the formation of a compound having the formula;

where R 3 is selected from

where R 4 is C 1 -C 4 alky, aryl or phenyl, and n is 1 or 2, and reacting Compound 18R under conditions effective to promote the formation of compound rac-1.

20 . A process of making a compound having the formula:

comprising reacting a compound having the formula;

under conditions effective to promote the formation of a compound having the formula

and reacting compound 8 under conditions effective to promote the formation of Compound 2.

21 . A process of making a compound having the formula:

comprising reacting a compound having the formula;

under conditions effective to promote the formation of Compound 28.

22 . A process of making a compound having the formula:

comprising reacting a compound having the formula;

under conditions effective to promote the formation of compound rac-1.

23 . A process of making a compound having the formula:

comprising reacting a compound having the formula;

under conditions effective to promote the formation of Compound 29.

24 . A process of making a compound having the formula:

comprising reacting a compound having the formula;

under conditions effective to promote the formation of compound rac-1.

25 . A process of making a compound having the formula:

comprising reacting a compound having the formula

where each R 5 is selected from the group consisting of hydrogen, t-butoxycarbonyl, carboxybenzyl, para-methoxybenzylcarbonyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, benzyl, 9-fluorenylmethyloxycarbonyl, N-phthalimide, COCH 3 and COCF 3 , under conditions effective to promote the formation of Compound 2.

26 . A process of making a compound having the formula:

comprising reacting a compound having the formula

where R 3 is selected from the group consisting of

where R 4 is C 1 -C 4 alky, aryl or phenyl, and n is 1 or 2, under conditions effective to promote the formation of compound rac-1.

27 . A process of making a compound having the formula:

where R 6 is selected from the group consisting of C 1 -C 4 alkyl, benzyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, 3,4-dimethoxybenzyl, tert-butyldimethylsilyl, tert-butyldiphenylsilyl, and triisopropylsilyl,

comprising reacting a compound of formula

under conditions effective to promote the formation of compound 7R.

28 . A process of making a compound having the formula:

where R 6 is selected from the group consisting of C 1 -C 4 alkyl, benzyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, 3,4-dimethoxybenzyl, tert-butyldimethylsilyl, tert-butyldiphenylsilyl, and triisopropylsilyl,

comprising reacting a compound of formula

under conditions effective to promote the formation of compound 7R.

29 . A compound having the following formula:

where R 6 is selected from the group consisting of C 1 -C 4 alkyl, benzyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, 3,4-dimethoxybenzyl, tert-butyldimethylsilyl, tert-butyldiphenylsilyl, and triisopropylsilyl.

30 . A compound according to claim 5 , wherein R 6 is CH 3 .

31 . A process of making a compound having the formula:

where R 6 is selected from the group consisting of C 1 -C 4 alkyl, benzyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, 3,4-dimethoxybenzyl, tert-butyldimethylsilyl, tert-butyldiphenylsilyl, and triisopropylsilyl,

comprising reacting a compound of formula

under conditions effective to promote the formation of Compound 22R.

32 . A compound having the following formula:

where each R 5 is independently selected from the group consisting of hydrogen, t-butoxycarbonyl, carboxybenzyl, para-methoxybenzylcarbonyl, para-methoxybenzyl, 2,4-dimethoxybenzyl, benzyl, 9-fluorenylmethyloxycarbonyl, N-phthalimide, COCH 3 and COCF 3 .

33 . A compound of claim 32 having the following formula:

Assignments (3)
RELEASE OF SECURITY INTEREST Recorded Aug 31, 2017
From: BARCLAYS BANK PLC, AS COLLATERAL AGENT
To: ALBANY MOLECULAR RESEARCH, INC.; ALO ACQUISITION LLC; AMRI BURLINGTON, INC.; AMRI RENSSELAER, INC.; CEDARBURG PHARMACEUTICALS, INC.; OSO BIOPHARMACEUTICALS MANUFACTURING, LLC; AMRI SSCI, LLC; EUTICALS INC.
Reel/Frame 043742/0085 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2016
From: BRISTOL-MYERS SQUIBB COMPANY
To: ALBANY MOLECULAR RESEARCH, INC.
Reel/Frame 039116/0827 →
SECURITY INTEREST Recorded Aug 5, 2015
From: ALBANY MOLECULAR RESEARCH, INC.; AMRI SSCI, LLC
To: BARCLAYS BANK PLC, AS THE COLLATERAL AGENT
Reel/Frame 036257/0914 →