IP Library Granted Patent US 9,108,990
Granted Patent B2
US 9,108,990 · App. 14/227,308 · Granted Aug 18, 2015

Cyclopropyl MIDA boronate

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Quick Facts
Patent No.
US 9,108,990
App. No.
14/227,308
Granted
Aug 18, 2015
Kind
B2
Abstract

This disclosure concerns a protected cyclopropylboronic acid comprising a substituted cyclopropyl group and a boronic ester group having a protecting group. The protecting group is an N-methyliminodiacetic acid (MIDA) group or MIDA-based group.

Claims (39)

1. A method of forming a compound of formula I:

wherein

R 1 is selected from hydrogen, alkyl, substituted alkyl, alkenyl, substituted alkenyl, alkynyl, substituted alkynyl, aryl, and heteroaryl; and

R 2a , R 2b , R 2c , and R 2d are independently selected from hydrogen, alkyl, substituted alkyl, halogen, hydroxyl, cyano, phosphate, alkoxy, substituted alkoxy, carboxyl, carboxyl ester, heterocyclyl, substituted heterocyclyl, alkenyl, substituted alkenyl, amino, substituted amino, acyl, acylamino, aminoacyl, alkoxycarbonylamino, thiol, alkylthiol, substituted thioalkoxy, and sulfonyl,

wherein at least one of R 2a , R 2b , R 2c , and R 2d is not hydrogen;

comprising reacting a compound of formula 3a:

with a compound of formula 3b:

2. The method of claim 1 , wherein R 1 is alkyl.

3. The method of claim 1 , wherein one of R 2a , R 2b , R 2c , and R 2d is substituted alkyl and the others are hydrogen.

4. The method of claim 1 , wherein one of R 2a , R 2b , R 2c , and R 2d is trifluoromethyl and the others are hydrogen.

5. The method of claim 4 , wherein the compound of formula I has a trans stereochemistry with respect to the cyclopropyl ring.

6. A method of forming a compound of formula 4c:

wherein

R 2a , R 2b , R 2c , and R 2d are independently selected from hydrogen, alkyl, substituted alkyl, halogen, hydroxyl, cyano, phosphate, alkoxy, substituted alkoxy, carboxyl, carboxyl ester, heterocyclyl, substituted heterocyclyl, alkenyl, substituted alkenyl, amino, substituted amino, acyl, acylamino, aminoacyl, alkoxycarbonylamino, thiol, alkylthiol, substituted thioalkoxy, and sulfonyl,

wherein at least one of R 2a , R 2b , R 2c , and R 2d is not hydrogen;

comprising reacting a compound of formula 4a:

with a compound of formula 4b:

7. The method of claim 6 , wherein one of R 2a , R 2b , R 2c , and R 2d is substituted alkyl and the others are hydrogen.

8. The method of claim 6 , wherein one of R 2a , R 2b , R 2c , and R 2d is trifluoromethyl and the others are hydrogen.

9. The method of claim 8 , wherein the compound of formula 4c has a trans stereochemistry with respect to the cyclopropyl ring.

10. A method of forming a compound of formula 5c:

wherein

R 2a , R 2b , R 2c , and R 2d are independently selected from hydrogen, alkyl, substituted alkyl, halogen, hydroxyl, cyano, phosphate, alkoxy, substituted alkoxy, carboxyl, carboxyl ester, heterocyclyl, substituted heterocyclyl, alkenyl, substituted alkenyl, amino, substituted amino, acyl, acylamino, aminoacyl, alkoxycarbonylamino, thiol, alkylthiol, substituted thioalkoxy, and sulfonyl,

wherein at least one of R 2a , R 2b , R 2c , and R 2d is not hydrogen;

comprising reacting a compound of formula 5a:

wherein

each R is independently an alkyl or taken together with the atoms to which they are attached are a cyclic pinacolato boronate ester,

with a compound of formula 5b:

wherein

R 1 is selected from H, Li, Na and K.

11. The method of claim 10 , wherein each R is independently selected from methyl, n-propyl, isopropyl and n-butyl.

12. The method of claim 10 , wherein the R substituents taken together with the atoms to which they are attached are a cyclic pinacolato boronate ester.

13. The method of claim 10 , wherein R 1 is Na.

14. The method of claim 10 , wherein one of R 2a , R 2b , R 2c , and R 2d is substituted alkyl and the others are hydrogen.

15. The method of claim 10 , wherein one of R 2a , R 2b , R 2c , and R 2d is trifluoromethyl and the others are hydrogen.

16. The method of claim 15 , wherein the compound of formula 5c has a trans stereochemistry with respect to the cyclopropyl ring.

17. The method of claim 10 , wherein the reacting occurs in a polar aprotic solvent.

18. The method of claim 17 , wherein the polar aprotic solvent is DMSO or DMF.

19. The method of claim 10 , further comprising heating the polar aprotic solvent.

Assignments (3)
SECURITY INTEREST Recorded May 8, 2026
From: RIGEL PHARMACEUTICALS, INC.
To: MIDCAP FUNDING IV TRUST
Reel/Frame 075576/0880 →
SECURITY INTEREST Recorded Aug 25, 2022
From: RIGEL PHARMACEUTICALS, INC.
To: MIDCAP FINANCIAL TRUST
Reel/Frame 061327/0712 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 27, 2014
From: DUNCTON, MATTHEW; SINGH, RAJINDER
To: RIGEL PHARMACEUTICALS, INC.
Reel/Frame 033199/0505 →