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Preparation method of benazepril intermediate

An intermediate, hydrochloric acid technology, applied in the field of preparation of benazepril intermediates, can solve the problems of low product purity and low BTB yield of benazepril intermediates, and achieve simple operation, suitable for industrialization promotion, good The effect of economic benefits

Pending Publication Date: 2022-01-21
湖北德曦辰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is: the benazepril intermediate BTB productive rate that existing method synthesizes is low, the problem that product purity is not high

Method used

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  • Preparation method of benazepril intermediate
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  • Preparation method of benazepril intermediate

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preparation example Construction

[0021] Specifically, the present invention provides a preparation method of a benazepril intermediate BTB, comprising the following steps:

[0022] a, take butyrolactone, benzene, aluminum trichloride, hydrochloric acid as raw materials, prepare tetralone TNK; The concrete preparation process includes: (1) in the synthesis reactor, mix 500ml of benzene with 300g of anhydrous aluminum trichloride Mix, stir for 1-5h, then add 52g of butyrolactone dropwise, the dropwise temperature is 15-20℃, the dropwise time is 2-6h, after the dropwise addition is completed, stir for 1-3h; the temperature is raised to reflux, and the reflux temperature is kept for 3-8h , cooled to room temperature; (2) add 1500ml water and 200g hydrochloric acid to the ice separation kettle, turn on stirring after cooling to 0-5 ℃, and then slowly drop the material in the synthesis kettle into the ice separation kettle, and the temperature during ice separation ≤10℃; stir for 1 hour, stop stirring, let stand fo...

Embodiment 1

[0043] Embodiment 1 adopts the inventive method to prepare BTB high-quality goods

[0044] The specific operation steps are as follows:

[0045] a, take butyrolactone, benzene, aluminum trichloride, hydrochloric acid as raw material, prepare tetralone TNK; Concrete preparation process comprises: (1) 500ml benzene is mixed with 300g anhydrous aluminum trichloride in synthesis kettle , stirred for 1h, then added dropwise 52g of butyrolactone, the dropwise addition temperature was 15°C, and the dropwise addition time was 2h. After the dropwise addition was completed, stirred for 1h; heated to reflux, kept at reflux for 3h, and cooled to room temperature; Add 1500ml of water and 250g of hydrochloric acid into the kettle, and start stirring after cooling down to 0°C, then slowly add the materials in the synthesis kettle to the ice-out kettle, the temperature during ice-out is ≤10°C; stir for 1 hour, stop stirring, and let stand For half an hour, remove the lower water layer; add 7...

Embodiment 2

[0055] Embodiment 2 adopts the inventive method to prepare BTB high-quality goods

[0056] The specific operation steps are as follows:

[0057] a, take butyrolactone, benzene, aluminum trichloride, hydrochloric acid as raw material, prepare tetralone TNK; Concrete preparation process comprises: (1) 500ml benzene is mixed with 300g anhydrous aluminum trichloride in synthesis kettle , stirred for 5 hours, then added dropwise 52g of butyrolactone, the dropwise addition temperature was 20°C, and the dropwise addition time was 6h. After the dropwise addition was completed, stirred for 3h; the temperature was raised to reflux, kept at reflux for 8h, and cooled to room temperature; Add 1500ml of water and 250g of hydrochloric acid into the kettle, start stirring after cooling down to 5°C, then slowly add the materials in the synthesis kettle dropwise to the ice-out kettle, the temperature during ice-out is ≤10°C; stir for 1 hour, stop stirring, and let stand For half an hour, remov...

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of a benazepril intermediate. In order to solve the problems of low yield and low product purity of the benazepril intermediate BTB synthesized by the existing method, the invention provides a preparation method of the benazepril intermediate BTB. Butyrolactone, benzene, aluminum trichloride and hydrochloric acid are adopted as raw materials, tetralone TNK is firstly prepared, and then a refined product of the benazepril intermediate BTB is prepared through oximation reaction and rearrangement reaction. The raw materials are easy to obtain, the method is easy to operate, the purity of the prepared benazepril intermediate BTB product reaches 99.5%, the yield is larger than 90%, and compared with an existing method for preparing the benazepril intermediate BTB, the method is better, and the method is suitable for application and popularization.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of a benazepril intermediate. Background technique [0002] Hypertension is a common disease in modern society. With the improvement of living standards, people eat more and more oil and fat, and the risk of hypertension is gradually increasing. At present, the main drugs for the treatment of hypertension are angiotensin-converting enzyme inhibitors. And benazepril, the chemical name is (3s)-3-{[((1s)-1-ethoxycarbonyl)-3-phenylpropyl]amino}-2,3,4,5-tetrahydro- 2-oxo-1H-1-benzoazepine-1-acetic acid, mp 148-149°C. [α] D-159° (C=1.2, ethanol). As a prodrug, it is rapidly absorbed, and is mainly converted into the active metabolite benazeprilat in the liver to inhibit angiotensin. It is a highly effective drug for the treatment of hypertension. [0003] At present, there are many preparation methods for the drug benazepril, and a variety of benazepr...

Claims

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Application Information

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IPC IPC(8): C07D223/16
CPCC07D223/16
Inventor 徐志谢忠杨
Owner 湖北德曦辰科技有限公司
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