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

A chemical synthesis, methoxyl technology, applied in the direction of organic chemistry, etc., can solve the problems of long reaction process time, incomplete reaction, low reaction yield, etc. The effect of cycle shortening

Active Publication Date: 2009-05-06
ZHEJIANG JIUZHOU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Therefore, in these two routes of above-mentioned A, B, all there is the problem that reaction process time is long, reaction yield is low, especially uses sodium methylate in B route, has the shortcoming of incomplete reaction, product yield is low

Method used

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

Examples

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Embodiment 1

[0030] Add 250ml of methanol into a 2000ml flask, then add 115g of KOH, and heat up to reflux until dissolved. Add 1200ml of toluene, add 65g of 10,11-dibromoiminodibenzyl, heat and reflux for 6-8 hours; add 300ml of water and stir, wash with water, let stand to remove the water layer, distill about 250ml of toluene under reduced pressure, cool and crystallize, Filter and dry to obtain 30.0 g of refined 10-methoxy-5H-dibenzo[b,f]azepine, with a yield of 85.8%.

Embodiment 2

[0032] Add 50ml of methanol to a 1000ml flask, then add 120g of CH 3 OK (supplier: Zibo Fuxier Chemical Co., Ltd.), heat up and reflux until dissolved. Add 500ml of toluene, put in 55g of 10,11-dibromoiminodibenzyl, heat and reflux for 6-8 hours; add 300ml of water and stir, wash with water, let stand to remove the water layer, distill about 120ml of toluene under reduced pressure, cool and crystallize, Filter and dry to obtain 24.1 g of refined 10-methoxy-5H-dibenzo[b,f]azepine, with a yield of 81.7%.

Embodiment 3

[0034] Add 250ml of methanol into a 1000ml flask, then add 200g of KOH, and heat up to reflux until dissolved. Add 120ml of xylene, put in 105g of 10,11-dibromoiminodibenzyl, heat and reflux for 6-8 hours; add 300ml of water and stir, wash with water, let stand to remove the water layer, evaporate about 30ml of xylene under reduced pressure, cool and analyze crystal, filtered, and dried to obtain 47.3 g of refined 10-methoxy-5H-dibenzo[b,f]azepine, with a yield of 84.2%.

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Abstract

The invention provides a method for chemically synthesizing 10-methoxyl-5H-dibenz [b, f] azapine. The 10-methoxyl-5H-dibenz[b, f] azapine is generated through reaction of 10, 11-iminodibenzyl dibromide and alkali metal hydroxide or alkali metal alcoholate in a mixed solvent; preferably, the mixed solvent comprises methanol and an aromatic solvent; the alkali metal hydroxide is selected from potassium hydroxide; and the alkali metal alcoholate is selected from potassium methoxide. The method comprises the following steps: firstly, adding the potassium hydroxide or the potassium methoxide to the methanol; adding the aromatic solvent and the 10, 11-iminodibenzyl dibromide to the mixed solvent after heating up and refluxing; performing heating, refluxing and preserving temperature for 6 to 8 hours; mixing and washing the mixed solvent by water, keeping the mixed solvent stand to remove an aqueous layer; decompressing and evaporating the solvent, cooling and chromatographing to the solvent, and filtering and drying the solvent to obtain pure 10-methoxyl-5H-dibenz[b, f] azapine. The method has the advantages of reasonable process, short reaction time and high reaction yield, and is applicable to 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. [0005] At present, the chemical synthesis methods of 10-methoxy-5H-dibenzo[b,f]azepine mainly contain the following two routes: [0006] A. British Patent GB 943277, date of announcement: December 4, 1963, named: 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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