Method for preparing escitalopram bis-hydroxynaphtoate crystal form a

Patent metadata

Field	Value
Publication number	US-12084425-B2
Application number	US-201917295843-A
Country	US
Kind code	B2
Filing date	Oct 12, 2019
Priority date	Nov 26, 2018
Publication date	Sep 10, 2024
Grant date	Sep 10, 2024

Abstract

Provided herein is a method for preparing an Escitalopram bis-hydroxynaphtoate ((S)-(+)-1-(3-(-(dimethylamino)propyl)-1-(4-fluorophenyl)-1,3-dihydro-5-cyanisob enzofuranone) crystal form A. Said method is ecofriendly and non pollutive, and the obtained Escitalopram bis-hydroxynaphtoate crystal form A is highly pure and easy to reproduce.

First claim

The invention claimed is:

1. A method for preparing a crystal form A of a compound of formula I, comprising:
dissolving escitalopram oxalate in a reaction solvent to obtain an escitalopram oxalate solution;
and adding a solution of a pamoate salt dropwise to precipitate the crystal form A of the compound of formula I

2. The method according to claim 1 , wherein the reaction solvent is water.

3. The method according to claim 1 , wherein dissolving is carried out at a temperature of 0-70° C.

4. The method according to claim 3 , wherein dissolving is carried out at a temperature of 25-35° C.

5. The method according to claim 1 , wherein the pamoate salt is disodium pamoate.

6. The method according to claim 1 , wherein a solvent of the solution of the pamoate salt is a mixed solvent of water and ethanol.

7. The method according to claim 6 , wherein a volume ratio of water and ethanol in the mixed solvent is 7:3-3:7.

8. The method according to claim 1 , wherein during adding the solution of the pamoate salt dropwise, a temperature of the escitalopram oxalate solution is 25-35° C.

9. The method according to claim 8 , wherein during adding the solution of the pamoate salt dropwise, the temperature of the escitalopram oxalate solution is 30° C.

10. The method according to claim 1 , wherein a mass ratio of escitalopram oxalate and the pamoate salt is 1:0.9-1:1.2.

11. The method according to claim 1 , wherein the crystal form A of the compound of formula I has a X-ray powder diffraction spectrum, showing characteristic peaks at 8.9±0.2°, 11.3±0.2°, 13.2±0.2°, 18.4±0.2°, 20.6±0.2° and 21.9±0.2°.

12. The method according to claim 6 , wherein a volume ratio of water and ethanol in the mixed solvent is 1.2:1-1:1.2.

13. The method according to claim 6 , wherein a volume ratio of water and ethanol in the mixed solvent is 1:1.

Assignees

• Zhejiang Huahai Pharm Co Ltd
• Shanghai Aobo Pharmtech Inc Ltd

Inventors

• Xu Wei
• Chen Xi
• Gu Hong

Classifications

• C07B2200/13

  Crystalline forms, e.g. polymorphs · CPC title

• C07D307/87 Primary

  Benzo [c] furans; Hydrogenated benzo [c] furans · CPC title

• C07C51/43

  by change of the physical state, e.g. crystallisation · CPC title

• C07C51/412

  by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part · CPC title