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Method for synthesizing diethyl (tosyloxy)methylphosphonate

A technology of diethyl toluenesulfonyloxymethylphosphonate and diethyl phosphite is applied in the field of synthesizing diethyl p-toluenesulfonyloxymethylphosphonate, which can solve the problems of unsuitability for industrialization, troublesome post-processing and environmental protection High pressure and other problems, to achieve the effect of simple post-processing, short reaction time, and low environmental protection pressure

Inactive Publication Date: 2018-12-18
山东沾化永浩医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The present invention provides a method for synthesizing diethyl p-toluenesulfonyloxymethylphosphonate aimed at the above-mentioned defects, which solves the problem of low purity, low yield, complicated process, troublesome post-processing and environmental protection pressure in the existing technology. Large, not suitable for industrialization and other shortcomings

Method used

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  • Method for synthesizing diethyl (tosyloxy)methylphosphonate
  • Method for synthesizing diethyl (tosyloxy)methylphosphonate
  • Method for synthesizing diethyl (tosyloxy)methylphosphonate

Examples

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Embodiment 1

[0034] (1) In a 500ml three-neck flask, add 50g of 37% formaldehyde solution, 3.0g of sodium carbonate, cool down to 0°C, add 60g of diethyl phosphite dropwise, and keep the temperature between 0-5°C during the dropping process , The addition was completed in 2 hours, and after the addition was completed, the reaction solution was obtained by incubating at 2°C for 2 hours. Sampling detection, diethyl phosphite 0.12% (less than 0.2%), the reaction is complete.

[0035] (2) Add 100 milliliters of methylene chloride and 78.7 grams of p-toluenesulfonyl chloride to the above reaction solution, cool down to 5° C., add 63.8 grams of 30% liquid caustic soda dropwise, the reaction is exothermic, and keep the dropping temperature between 5-10° C. , after adding in 1 hour, after the dropwise addition, keep warm at 10°C for 2 hours, take a sample test, the reaction of p-toluenesulfonyl chloride 0.15% (less than 0.2%) is completed, stand still, separate layers, add 50 ml of dichloromethane...

Embodiment 2

[0048] (1) In a 500 ml three-necked flask, add 55 grams of 37% formaldehyde solution, 3.0 grams of sodium carbonate, cool down to 0°C, add 60 grams of diethyl phosphite dropwise, and keep the temperature during the dropping process between 0-5°C , The addition was completed in 2 hours, and after the addition was completed, the reaction solution was obtained by incubating at 2°C for 2 hours. Sampling detection, diethyl phosphite 0.11% (less than 0.2%), the reaction is complete.

[0049] (2) Add 100 milliliters of methylene chloride and 78.7 grams of p-toluenesulfonyl chloride to the above reaction solution, cool down to 5° C., add 63.8 grams of 30% liquid caustic soda dropwise, the reaction is exothermic, and keep the dropping temperature between 5-10° C. , Added in 1 hour, the dropwise addition was completed and kept at 10°C for 2 hours, sampling was detected, the reaction of p-toluenesulfonyl chloride 0.13% (less than 0.2%) was completed, static, separated, the water layer wa...

Embodiment 3

[0051] 1) In a 500 ml three-necked flask, add 50 grams of 37% formaldehyde solution, 3.0 grams of potassium carbonate, cool down to 0°C, add 60 grams of diethyl phosphite dropwise, and keep the temperature during the dropping process between 0-5°C. The addition was completed in 2 hours, and after the addition, it was incubated at 2°C for 2 hours to obtain a reaction solution. Sampling detection, diethyl phosphite 0.09% (less than 0.2%), the reaction is complete.

[0052](2) Add 100 milliliters of methylene chloride and 78.7 grams of p-toluenesulfonyl chloride to the above reaction solution, cool down to 5° C., add 63.8 grams of 30% liquid caustic soda dropwise, the reaction is exothermic, and keep the dropping temperature between 5-10° C. , after adding in 1 hour, after the dropwise addition, keep warm at 10°C for 2 hours, take a sample test, the reaction of p-toluenesulfonyl chloride 0.18% (less than 0.2%) is completed, stand still, separate layers, add 50 ml of dichlorometha...

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Abstract

The invention discloses a method for synthesizing diethyl (tosyloxy)methylphosphonate. The method comprises the following steps: mixing a 37% aqueous formaldehyde solution with a catalyst, dropwise adding diethyl phosphite, carrying out a heat insulation reaction for 2 h after the dropwise addition is completed in order to obtain a reaction solution, adding a solvent and p-toluenesulfonyl chlorideto the reaction solution, dropwise adding an acid binding agent at a low temperature, carrying out heat insulation for about 2 h after the dropwise addition is completed, performing extraction, washing the obtained reaction product with water, and distilling the washed reaction product to obtain a remaining material that is highly-pure for synthesizing diethyl (tosyloxy)methylphosphonate. The method overcomes the disadvantages of low purity, low yield, complicated process, troublesome post-treatment, large environmental protection pressure and unsuitability for industrialization in the priorart.

Description

technical field [0001] The invention relates to the technical field of medicine synthesis, in particular to a method for synthesizing diethyl p-toluenesulfonyloxymethylphosphonate. Background technique [0002] Diethyl p-toluenesulfonyloxymethylphosphonate is used in herbicides and fungicides, and another important use is as an intermediate in the synthesis of nucleoside antiviral drugs for the treatment of viral infectious diseases Tylenol fumarate Fuvir dipivoxil intermediate. The synthesis process of diethyl p-toluenesulfonyloxymethylphosphonate reported in the literature, the actual product purity is not high, the yield is low, the aftertreatment is complicated, the sewage treatment is difficult, and the production cost remains high. [0003] At present, the synthesis route of diethyl p-toluenesulfonyloxymethylphosphonate is relatively simple. Under the action of catalyst, diethyl phosphite and paraformaldehyde undergo addition reaction to obtain diethyl hydroxymethyl p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40
CPCC07F9/4006C07F9/4075
Inventor 倪政
Owner 山东沾化永浩医药科技有限公司
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