Process for synthesizing O,O'-alkyl thiophosphoric acid

A technology of an alkyl thiophosphoric acid and a synthesis method, applied in the field of O, can solve the problems of low yield, many by-products, accelerated side reactions, etc., and achieves high reaction yield, reduced possibility of accidents, and suppressed side reactions. Effect

Inactive Publication Date: 2005-11-30
姚文刚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantages are: 1. due to the high activity of phosphorus pentasulfide, the heat of reaction will accelerate the reaction itself and other side reactions of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Example 1, the preparation of O, O'-dimethylthiophosphoric acid: add 13 grams of methanol, 350 milliliters of benzene, and 5 grams of triethylamine in the reaction kettle, and control the temperature between 10 and 15°C under stirring. During this period, about 222 grams of phosphorus pentasulfide was put into it, and then 121 grams of methanol was added dropwise within 30 to 60 minutes while maintaining the temperature between 10 and 15°C, and continued to insulate and stir for 0 to 2 hours to obtain O, O'-dimethylphosphoric acid thioxate. The rate is about 98%.

Embodiment 2

[0009] Example 2 is the same as Example 1, and the temperature is controlled between 20-25°C to obtain O, O'-dimethylthiophosphoric acid with a yield of about 98%.

Embodiment 3

[0010] Example 3 is the same as Example 1, and the temperature is controlled between 35-40°C to obtain O, O'-dimethylphosphoric acid thio, with a yield of about 98%.

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PUM

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Abstract

The invention discloses a method for synthesizing O, O'-dialkyl phosphorothioic acid, which takes phosphorothioic acid and low-carbon alcohol as materials to synthesize O, O'-dialkyl phosphorothioic acid with the existing of catalyst and organic solvent. The invention chooses organic amine and tervalence organo-phosphines compound as catalyst and choose non-polar organics such as aromatics, alkyl halide and esters as organic solvent. The invention has the advantages of little side reaction, simple removal of reaction heat, low likelihood of accident and high yield.

Description

Technical field: [0001] The invention relates to a synthesis method of O, O'-alkylthiophosphoric acid, which belongs to the class of phosphorothioates. Background technique: [0002] Existing O, the synthetic method of O'-alkoxythiophosphoric acid, adopts under the condition that phosphorothioates exists usually, lower carbon alcohol is joined in phosphorus pentasulfide and reacts and obtains. For example, West German patent 2500452 reported the synthesis of O, O'-dimethylthiophosphoric acid in 1975. The method is: mix phosphorus pentasulfide with 15-18% neutral oil (reaction by-product), and heat A slight excess of methanol was added dropwise, and then the temperature was raised to 60° C., and reacted for 1 hour. The product was neutralized into sodium salt for use in the next step, and the yield was 75-80%. Its disadvantages are: 1. due to the high activity of phosphorus pentasulfide, the heat of reaction will accelerate the reaction itself and other side reactions of pho...

Claims

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Application Information

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IPC IPC(8): C07F9/16
Inventor 姚文刚
Owner 姚文刚
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