IP Library Granted Patent US 8,278,435
Granted Patent B2
US 8,278,435 · App. 12/968,110 · Granted Oct 2, 2012

N-pyrazole A2A receptor agonists

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Quick Facts
Patent No.
US 8,278,435
App. No.
12/968,110
Granted
Oct 2, 2012
Kind
B2
Abstract

The present disclosure provides a process for the preparation of 2-adenosine N-pyrazole compounds exemplified by the structure shown below that are potent and selective agonists for A 2A adenosine receptor, compositions comprising these compounds, and methods for using these compounds to stimulate mammalian coronary vasodilation for imaging the heart.

Claims (28)

1. A method for the preparation of (1-{9-[(4S,2R,3R,5R)-3,4-dihydroxy-5-(hydroxymethyl)oxolan-2-yl]-6-aminopurin-2-yl}pyrazol-4-yl)-N-methylcarboxamide:

comprising heating a compound of formula 10:

in excess methylamine to provide (1-{9-[(4S,2R,3R,5R)-3,4-dihydroxy-5-(hydroxymethyl)oxolan-2-yl]-6-aminopurin-2-yl}pyrazol-4-yl)-N-methylcarboxamide.

2. The method of claim 1 , wherein the method comprises an aqueous solution of methylamine.

3. The method of claim 1 , wherein the method comprises heating at a temperature of about 65° C.

4. The method of claim 1 , wherein the method comprises an aqueous solution of methylamine and heating at a temperature of about 65° C.

5. The method of claim 1 , wherein the method further comprises preparing the compound of formula 10:

by reacting a compound of formula 1:

with ethoxycarbonylmalondialdehyde.

6. The method of claim 5 , wherein preparing the compound of formula 10 comprises a temperature of about 80° C.

7. The method of claim 5 , wherein preparing the compound of formula 10 comprises a mixture of CH 3 OH and CH 3 COOH as a solvent.

8. The method of claim 7 , wherein the mixture of CH 3 OH and CH 3 COOH is in a 1:1 ratio.

9. The method of claim 5 , wherein preparing the compound of formula 10 comprises a temperature of about 80° C. and a 1:1 mixture of CH 3 OH and CH 3 COOH as a solvent.

10. The method of claim 5 , wherein the method further comprises preparing the compound of formula 1:

by reacting a compound of formula 9:

with hydrazine hydrate.

11. The method of claim 10 , wherein the method further comprises preparing the compound of formula 9:

by reacting a compound of formula 8:

with NH 3 .

12. The method of claim 11 , wherein the method further comprises preparing the compound of formula 8:

by reacting a compound of formula 7:

with CH 3 (CH 2 ) 4 ONO and CH 2 I 2 .

13. The method of claim 12 , wherein the method further comprises preparing the compound of formula 7:

by reacting a compound of formula 6:

with POCl 3 .

14. The method of claim 13 , wherein the method further comprises preparing the compound of formula 6:

by reacting guanosine:

with acetic anhydride.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 1, 2012
From: ZABLOCKI, JEFF A.; PALLE, VENKATA P.; ELZEIN, ELFAITH O.; BELARDINELLI, LUIZ
To: CV THERAPEUTICS, INC.
Reel/Frame 028701/0691 →
MERGER Recorded Aug 1, 2012
From: APEX MERGER SUB, INC.; CV THERAPEUTICS, INC.
To: GILEAD PALO ALTO, INC.
Reel/Frame 028701/0855 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 10, 2011
From: GILEAD PALO ALTO, INC.
To: GILEAD SCIENCES, INC.
Reel/Frame 026424/0925 →