Diethyl p-toluenesulfonyloxy methylphosphonate synthesis method

A technology of diethyl toluenesulfonyloxymethylphosphonate and diethyl hydroxymethylphosphonate is applied in the field of synthesis of diethyl p-toluenesulfonyloxymethylphosphonate, which can solve the problem of increasing cost, difficulty in Avoid problems such as excessive water content of diethyl hydroxymethyl phosphonate, and achieve the effect of saving energy consumption, reducing post-processing procedures, and high purity
CN105541910AInactive Publication Date: 2016-05-04SHANDONG JINCHENG PHARMA & CHEM
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
SHANDONG JINCHENG PHARMA & CHEM
Publication Date
2016-05-04
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to the technical field of medicine, and specifically relates to a synthesis method of diethyl p-toluenesulfonyloxy methylphosphonate. The method comprises the following steps: (1) diethyl hydroxymethylphosphonate is synthesized, wherein diethyl phosphite, a solvent, a catalyst and paraformaldehyde are sequentially added into a reactor; heating is carried out and a reaction is allowed; filtering is carried out after the reaction; the solvent is removed through distillation, and the remaining substance is diethyl hydroxymethylphosphonate; and (2) diethyl p-toluenesulfonyloxy methylphosphonate is synthesized, wherein diethyl hydroxymethylphosphonate prepared in the step (1) is cooled; dichloromethane and p-toluenesulfonyl chloride are added; an acid binding agent is dropped in, and stirring is continuous for 1.5-2.5h after dropping; heating is carried out and a reaction is allowed; after the reaction, extraction, water washing and distillation are carried out, and the remaining substance is a crude product; and purification is carried out, such that a diethyl p-toluenesulfonyloxy methylphosphonate product is obtained. The method provided by the invention has the advantages of low energy consumption, simple product post treatment, high yield and high product purity. The yield can be higher than 80%. The purity can be higher than 99%.
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Description

technical field

[0001] The invention belongs to the technical field of pharmaceutical synthesis, and in particular relates to a synthesis method of diethyl p-toluenesulfonyloxymethylphosphonate. Background technique

[0002] Diethyl p-toluenesulfonyloxymethylphosphonate can not only be used for herbicides and fungicides, but also an important intermediate for the synthesis of nucleoside antiviral drugs tenofovir disoproxil and adefovir dipivoxil. The synthesis process of diethyl toluenesulfonyloxymethylphosphonate has complex reaction conditions and incomplete product purification.

[0003] At present, the synthesis route of diethyl p-toluenesulfonyloxymethylphosphonate is relatively simple. With toluene as solvent, under the catalysis of triethylamine, diethyl phosphite and paraformaldehyde undergo addition reaction, and then molecular Internal rearrangement to obtain diethyl hydroxymethylphosphonate, p-toluenesulfonyl chloride is directly added to the reaction solution to...

Claims

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