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Method for preparing methodlene tetraethyl diphosphate

A technology of tetraethyl methylene diphosphonate and triethyl phosphite, which is applied in the field of preparing tetraethyl methylene diphosphonate, can solve the problems of low reaction yield and achieve high reaction yield and reaction stable effect

Active Publication Date: 2007-06-13
GUANGZHOU WISDOM BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is the shortcoming that reaction yield is low in above-mentioned method

Method used

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  • Method for preparing methodlene tetraethyl diphosphate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Measure 4ml (9.92g) of dibromomethane and mix with 30ml (29.05g) of triethyl phosphite. The mixture was heated to 100°C under reflux for 30 minutes, and then heated to 175°C for 22 hours. During the reaction, the by-product bromoethane is steamed out, and the unnecessary reactants and by-products are steamed by distillation under reduced pressure, and finally, distillation under reduced pressure obtains 13.6 g of product tetraethyl methylene diphosphonate (content reaches 95.4%), and the yield was 79.0%.

Embodiment 2

[0015] Measure 8 ml (19.8 g) of dibromomethane and mix with 60 ml (58.1 g) of triethyl phosphite. The mixture was heated to 90°C under reflux for 35 minutes, and then heated to 185°C for 18 hours. During the reaction, the by-product bromoethane was steamed out, and the unnecessary reactants and by-products were steamed by distillation under reduced pressure, and finally the product was distilled under reduced pressure to obtain 27.8 g (content of 95.2%) of tetraethyl methylene diphosphonate. was 80.8%.

Embodiment 3

[0017] Measure 16 ml (39.6 g) of dibromomethane and mix with 100 ml (97.4 g) of triethyl phosphite. The mixture was heated to 85° C. for reflux reaction for 40 minutes, and then heated to 190° C. for 20 hours. During the reaction, the by-product bromoethane was steamed out, and the unnecessary reactants and by-products were steamed by distillation under reduced pressure, and finally the product was distilled under reduced pressure to obtain 53.8 g of tetraethyl methylene diphosphonate (the content reached 95.8%), and the yield was 78.6%.

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Abstract

This invention relates to a preparation of methylene diphosphonate tetro-ethyl ester. Dibromomethane and triethyl phosphate are mixed according to gram-molecule ratio 1:2-1:3,then first progress low temperature reaction at 85-100 C degree about 30-40 minutes, and it is reheated to 175-190 C degree to progress hyperthermic response about 18-24 hours, condensed to prepare methylene diphosphonate tetro-ethyl ester.

Description

field of invention [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing tetraethyl methylene diphosphonate. Background technique [0002] Tetraethyl methylene diphosphonate is widely used as an important intermediate in the preparation of medicines and food additives, for example, it is an important intermediate for the preparation of 3-methyl-5-(2,6,6-trimethyl-1-cyclohexene- 1-yl)-1,3-pentadienyl phosphate diethyl ester, 3-methyl-5-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4- Diethyl pentadienyl phosphate, 3-methyl-5-(2,6,6-trimethyl-1-cyclohexen-1-yl)-1,3-dimethyl pentadienyl phosphate, 3 -Propyl-5-(2,6,6-trimethyl-1-cyclohexen-1-yl)-1,3-pentadienyl phosphate diethyl ester, 3-methyl-5-(2, 6,6-trimethyl-1-cyclohexen-1-yl)-1,3-di-tert-butyl pentadienyl phosphate, 3-ethyl-5-(2,6,6-trimethyl- An important intermediate of 1-cyclohexen-1-yl)-1,3-pentadienyl diisopropyl phosphate. Its structural formula is as follows...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40
Inventor 吴世林陆豫刘学辉
Owner GUANGZHOU WISDOM BIO TECH
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