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Chemical synthesis method of 10-methoxyl-5H-dibenz[b,f]azapine

A chemical synthesis, methoxy technology, applied in the direction of organic chemistry, can solve the problem of low reaction yield, and achieve the effect of increased yield, large implementation value and social and economic benefits

Active Publication Date: 2009-03-18
ZHEJIANG JIUZHOU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Like this, in these two routes of above-mentioned A, B, especially use sodium methylate in B route, there is the shortcoming that reaction yield is low

Method used

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  • Chemical synthesis method of 10-methoxyl-5H-dibenz[b,f]azapine

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Experimental program
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Embodiment 1

[0023] Add 500ml of methanol into a 1000ml flask, then add 175g of KOH, and heat up to reflux until dissolved. Add 100g of 10,11-dibromoiminodibenzyl, heat and reflux for 24 hours; evaporate methanol to dryness under reduced pressure, add 300ml of water, stir, filter, and dry to obtain 10-methoxy-5H-dibenzo[b,f ] Azapine crude product 48.4g, yield 90.1%;

[0024] Add 48.4 g of the crude product of 10-methoxy-5H-dibenzo[b, f]azepine to 200 ml of methanol, heat to dissolve, cool, crystallize, filter and dry to obtain 10-methoxy-5H-dibenzo[b,f] [b, f] 41.9g of azapine fine product, the refined yield is 78.0%.

Embodiment 2

[0026] Add 500ml of methanol into a 1000ml flask, then add 219g of CH3OK (supplier: Zibo Fuxier Chemical Co., Ltd.), heat up and reflux until dissolved. Add 100g of 10,11-dibromoiminodibenzyl, heat and reflux for 24 hours; evaporate methanol to dryness under reduced pressure, add 300ml of water, stir, filter, and dry to obtain 10-methoxy-5H-dibenzo[b,f ] Azapine crude product 47.1g, yield 87.6%;

[0027] Add 47.1 g of the crude product of 10-methoxy-5H-dibenzo[b, f]azepine to 200 ml of methanol, heat to dissolve, cool, crystallize, filter and dry to obtain 10-methoxy-5H-dibenzo[b,f] [b, f] 40.7g of azapine fine product, the refined yield is 75.7%.

[0028] In summary, the chemical synthesis method of 10-methoxy-5H-dibenzo[b,f]azepine of the present invention has reasonable process, high reaction yield and is suitable for large-scale industrial production.

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Abstract

The invention provides a method for chemically synthesizing 10-methoxy-5H-dibenzo[b, f]azepin. The method comprises the following steps: using 10, 11-dibromo-imino-dibenzyl as a raw material to react with potassium hydroxide or potassium methoxide in methanol so to generate the10-methoxy-5H-dibenzo[b, f]azepin; preferably, firstly, adding the potassium hydroxide or the potassium methoxide in the methanol, adding the 10, 11-dibromo-imino-dibenzyl into the mixture after heating up and refluxing the mixture, and reducing the pressure and distilling the methanol after heating up and refluxing the mixture as well as keeping the temperature for a period of time; secondly, adding water into the mixture, and stirring, filtering and drying the mixture to obtain a crude product of the 10-methoxy-5H-dibenzo[b, f]azepin; and finally, adding solvent into the crude product for refinement to obtain the refined product of the 10-methoxy-5H-dibenzo[b, f]azepin. The method has the advantages of reasonable process and high reaction yield, and suitability for large-scale industrial production.

Description

technical field [0001] The present invention relates to the technical field of 10-methoxyl-5H-dibenzo[b,f]azepine, more specifically, relates to the technical field of 10-methoxyl-5H-dibenzo[b,f]azepine The technical field of chemical synthesis, in particular, refers to a chemical synthesis method of 10-methoxy-5H-dibenzo[b,f]azepine. Background technique [0002] 10-methoxy-5H-dibenzo[b,f]azepine (10-methoxy-5H-dibenz[b,f]azepine), molecular formula: C 15 h 13 NO, molecular weight: 223.27, appearance is bright yellow crystalline powder, its structural formula is as follows: [0003] [0004] It is a chemical intermediate and has a very wide range of uses in the fields of chemical and pharmaceutical synthesis. At present, the chemical synthesis methods of 10-methoxy-5H-dibenzo[b,f]azepine mainly contain the following two routes: [0005] A. British Patent GB943277, the announcement date is: December 4, 1963, the name is: dibenzo [b, f] azepines and their preparation p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/22
Inventor 陈士明徐旭伟
Owner ZHEJIANG JIUZHOU PHARM CO LTD
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