IP Library Granted Patent US 9,546,137
Granted Patent B2
US 9,546,137 · App. 14/420,728 · Granted Jan 17, 2017

Methods of preparing Tecovirimat

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Quick Facts
Patent No.
US 9,546,137
App. No.
14/420,728
Granted
Jan 17, 2017
Kind
B2
Abstract

Disclosed are methods for the preparation of Tecovirimat for the treatment or prophylaxis of viral infections and diseases associated therewith, particularly those viral infections and associated diseases caused by the orthopoxvirus.

Claims (13)

1. A method for producing N-[(3aR,4R,4aR,5aS,6S,6aS)-3,3a,4,4a,5,5a,6,6a-octahydro-1,3-dioxo-4,6-ethenocycloprop[f]isoindol-2(1H)-yl]-4-(trifluoromethyl)-benzamide, said method comprising:

(a) reacting compound 3 of formula:

 with tert-butyl carbazate (compound 5) to form compound 6 of formula:

(b) reacting compound 6 with an acid to form compound 7 or salt thereof of formula:

(c) reacting compound 7 with 4-(trifluoromethyl)benzoyl chloride (compound 8); and

(d) collecting N-[(3aR,4R,4aR,5aS,6S,6aS)-3,3a,4,4a,5,5a,6,6a-octahydro-1,3-dioxo-4,6-ethenocycloprop[f]isoindol-2(1H)-yl]-4-(trifluoromethyl)-benzamide.

2. The method of claim 1 , wherein step (a) is carried under nitrogen atmosphere above room temperature.

3. The method of claim 1 , wherein said acid in step (b) is HCI.

4. The method of claim 1 , wherein compound 6 is dissolved in i-PrOAc prior to the reaction of step (b).

5. The method of claim 1 , wherein a base is present in the reaction of step (c), wherein said base is selected from the group consisting of: pyridine, 4-dimethylaminopyridine, triethylamine and diisopropylethylamine.

6. The method of claim 1 , wherein step (c) is carried out at a temperature of less than about 20° C.

7. The method of claim 1 , wherein said N-[(3aR,4R,4aR,5aS,6S,6aS)-3,3a,4,4a,5,5a,6,6a-octahydro-1,3-dioxo-4,6-ethenocycloprop[f]isoindol-2(1H)-yl]-4-(trifluoromethyl)-benzamide collected in step (d) is further purified by column chromatography.

8. Compound 6 of the following formula:

Assignments (3)
RELEASE OF SECURITY INTEREST IN INTELLECTUAL PROPERTY AT REEL/FRAME NO. 40349/0219 Recorded Mar 13, 2020
From: CORTLAND CAPITAL MARKET SERVICES LLC
To: SIGA TECHNOLOGIES, INC.
Reel/Frame 052163/0014 →
SECURITY INTEREST Recorded Nov 16, 2016
From: SIGA TECHNOLOGIES, INC.
To: CORTLAND CAPITAL MARKET SERVICES, LLC
Reel/Frame 040349/0219 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 10, 2015
From: DAI, DONGCHENG
To: SIGA TECHNOLOGIES, INC.,
Reel/Frame 034928/0011 →