Aftertreatment purification method for 3-[(3-amino-4-methylamino benzoyl)(pyridine-2-yl)amino]ethyl propionate

A technology of methylaminobenzoyl and ethyl propionate, which is applied in the field of post-treatment purification of pharmaceutical intermediates 3-[amino] ethyl propionate and 3-[amino] ethyl propionate, and can solve post-treatment purification The method process is complicated, the product properties are not very good, and it is uneconomical, etc., to achieve significant creativity and practical value, improve production safety, and be easy to operate.
CN104892501AInactive Publication Date: 2015-09-09SHANGHAI INST OF TECH
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Patent Information

Authority / Receiving Office
CN ยท China
Patent Type
Applications(China)
Current Assignee / Owner
SHANGHAI INST OF TECH
Publication Date
2015-09-09
Estimated Expiration
Not applicable ยท inactive patent

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Abstract

The invention discloses an aftertreatment purification method for 3-[(3-amino-4-methylamino benzoyl)(pyridine-2-yl)amino]ethyl propionate. The method comprises the following steps: reducing 3-[(3-nitro-4-methylamino benzoyl)(pyridine-2-yl)amino]ethyl propionate hydrochloride with metal zinc in an acetic acid / water system so as to obtain a mother solution; and filtering and washing the mother solution, regulating the PH of the mother solution with alkali liquor, extracting the mother solution with a first organic solvent, condensing, dissolving the mother solution with a second organic solvent, absorbing by use of silica gel, eluting with a third organic solvent, and condensing to obtain a white solid, namely 3-[(3-amino-4-methylamino benzoyl)(pyridine-2-yl)amino]ethyl propionate. According to the aftertreatment purification method, a silica gel adsorption method and an eluting method are adopted to remove pigments and byproducts generated in reaction, so that aftertreatment is simple, the target organic product purity is improved and a high-purity target compound is obtained.
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Description

technical field

[0001] The invention belongs to the field of medicinal chemistry, in particular to a pharmaceutical intermediate 3-[(3-amino-4-methylaminobenzoyl)(pyridin-2-yl)amino]ethyl propionate, specifically a 3-[(3-Amino-4-methylaminobenzoyl)(pyridin-2-yl)amino]propanoic acid ethyl ester post-treatment purification method. Background technique

[0002] Ethyl 3-[(3-amino-4-methylaminobenzoyl)(pyridin-2-yl)amino]propionate (compound (1)) is a key intermediate for the preparation of dabigatran etexilate. Dabigatran etexilate (English name Dabigatranetexilate, compound (2)) is a new type of direct thrombin inhibitor. This drug was invented by Boehringer Ingelheim of Germany, and it was first launched in Germany and the UK in April 2008. This is the first new class of oral anticoagulant drug launched in the past 50 years after warfarin.

[0003]

[0004] In the prior art, such as CN102612517A, the synthetic route of dabigatran etexilate is shown in formula 1:

[0005] ...

Claims

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