IP Library Granted Patent US 8,993,762
Granted Patent B2
US 8,993,762 · App. 13/840,975 · Granted Mar 31, 2015

Total synthesis of thaxtomin A analogues and their intermediates

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Quick Facts
Patent No.
US 8,993,762
App. No.
13/840,975
Granted
Mar 31, 2015
Kind
B2
Abstract

Improved synthetic methods for the production of thaxtomin analogs, particularly thaxtomin A, and intermediates therefore such as substituted tryptophans and in particular, 4-nitro-L-tryptophan, and substituted phenyl acrylic acids are disclosed. Bioassays show that the synthetic thaxtomin A is not significantly different from the natural one in herbicidal activity.

Claims (15)

1. A method for the synthesis of a thaxtomin or analog thereof having the structure (I)

wherein R1 is NO 2 and R2 is selected from a lower alkyl, hydroxyl, halogen, fluoromethyl, difluoromethyl, trifluoromethyl, nitro, amine, methoxy, fluoromethoxy, difluoromethoxy, and trifloromethoxy, comprising:

(a) reacting a tryptophan amide analog having the structure

with substituted phenyl acrylic acid having the structure

wherein R is selected from a lower alkyl, hydroxyl, halogen, fluoromethyl, difluoromethyl, trifluoromethyl, nitro, amine, methoxy, fluoromethoxy, difluoromethoxy, and trifloromethoxy, or its keto tautomer to obtain a compound having the structure (A2)

wherein R1 is NO 2 and R2 is selected from a lower alkyl, hydroxyl, halogen, fluoromethyl, difluoromethyl, trifluoromethyl, nitro, amine, methoxy, fluoromethoxy, difluoromethoxy, and trifloromethoxy; and

(b) subjecting the compound having the structure (A2) to a cyclization agent to obtain the structure (I).

2. The method according to claim 1 , wherein said thaxtomin analogue is thaxtomin A having the structure

3. The method according to claim 1 , wherein said substituted phenylacrylic acid has the structure

wherein R is OH or its keto tautomer.

4. The method according to claim 3 , wherein said substituted phenylacrylic acid has the structure

5. The method according to claim 1 , wherein the cyclization is by means of an organic base.

6. The method according to claim 5 wherein the organic base is potassium hydroxide.

7. The method according to claim 5 , wherein the organic base is a chiral Lewis base.

8. The method according to claim 5 wherein the organic base is selected from the group consisting of substituted or unsubstituted pyridine, amine, imidazole, benzimidazole, histidine, and phosphazene.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 28, 2026
From: WILMINGTON SAVINGS FUND SOCIETY, FSB
To: PFG HOLDING CORPORATION
Reel/Frame 075515/0294 →
RELEASE OF SECURITY INTEREST Recorded Aug 10, 2022
From: IVY INVESTMENT MANAGEMENT COMPANY
To: PRO FARM GROUP, INC.
Reel/Frame 061067/0536 →
INTELLECTUAL PROPERTY SECURITY AGREEMENT Recorded Aug 21, 2015
From: MARRONE BIO INNOVATIONS, INC.
To: IVY INVESTMENT MANAGEMENT COMPANY
Reel/Frame 036420/0429 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 30, 2013
From: HUANG, HUAZHANG; YAN, DONG; XUE, ZHIJIE; ZHANG, HONGBO
To: MARRONE BIO INNOVATIONS, INC.
Reel/Frame 031509/0614 →