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Direct electrochemical synthesis method of thiophosphate compound

A technology of phosphorothioate and synthesis method, which is applied in the direction of electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of high raw material price and long reaction time, and achieve the effect of reducing environmental cost and good universality

Active Publication Date: 2021-06-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent (CN10884260) has reported a kind of method of phosphite triester and disulfide reaction to prepare phosphorothioate compound, and reaction does not need catalyst or promotor; But this reaction can only be applicable to diaryl disulfide substrate , and disulfide compounds still need to be prepared from mercaptans as raw materials
The above methods have their own advantages, but they also have their own shortcomings. For example, some methods need to use stoichiometric oxidants, some methods have limited substrates, some methods require relatively high raw material prices, and some methods require long reaction times.

Method used

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  • Direct electrochemical synthesis method of thiophosphate compound
  • Direct electrochemical synthesis method of thiophosphate compound
  • Direct electrochemical synthesis method of thiophosphate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: O, O-diethyl-S - pair of phenylthio phosphate (preparation of formula (I-1))

[0022] Add 0.1mol / L bu in 30 ml of beakers 4 NBF 4 Ethyl acetonitrile solution (15 mL), triethylate (0.5 mmol) and toluene (0.9 mmol). 40 ° C, 1.0V disperse potential electrolysis, the reaction is completed after 4 hours. The solvent was evaporated under reduced pressure, and the column chromatography was separated, and the mixture of petroleum ether / ethyl acetate was 8: 1, the eluent containing the target compound was collected, and the solvent was evaporated. O-diethyl-S-p-p-phenylthio phosphate, separated yield is 68%.

Embodiment 2

[0023] Example 2: O, O-diethyl-S - pair of phenylthio phosphate (formula (I-1))

[0024] The reaction step is in Example 1, and the difference is 0.9 mmol, O, O-diethyl-S-S-Diethyl-S-S-S-Diethyl-S-S-Si-S-Diethyl-S- 55%.

Embodiment 3

[0025] Example 3: O, O-diethyl-S - preparation of toluene thiophosphate (formula (I-1))

[0026] The reaction step is the same as in Example 1, which is 0.75 mmol, O, O-diethyl-S-Di-sulphophosphate, is 51%.

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Abstract

The invention discloses a direct electrochemical synthesis method of a thiophosphate compound. A three-electrode system is adopted in the reaction, a cathode and an anode are Pt electrodes, and a 0.1 mol / L silver nitrate acetonitrile solution is used as a reference electrode; triester phosphite and mercaptan are added into a Bu4NBF4 acetonitrile solution with a certain concentration, stirring and electrolytic reaction are conducted for 2-6 hours under the conditions that the temperature is 25-55 DEG C and the constant pressure is 0.6-1.4 V, and after the reaction is finished, separation treatment is conducted to obtain the thiophosphate compound. According to the synthesis method disclosed by the invention, clean electric energy is used as an oxidizing agent, so that the environmental cost is reduced; and the universality of the reaction substrate is good.

Description

Technical field [0001] The present invention belongs to the field of organic synthesis, and more particularly to a direct electrochemical synthesis method of a phosphate compound. Background technique [0002] The organic compounds containing phosphorus and sulfur are special and widely used in the molecule. The phosphate compound is an important such as a sulfur phosphorus organic compound, which has a wide range of uses in various fields such as pharmaceutical, pesticides, biology, and materials. The synthesis of such a conventional compound is made of halogenate and thiol as a raw material, but the halogenated phosphate compound has been complex and is inconvenient. In recent years, a method of synthesizing a phosphate compound by a CDC reaction is gradually attracted by a CDC to synthesize a phosphorite compound by a CDC, and the literature has more reported. [0003] The price of trigsterine compounds of phosphite is inexpensive, and the nucleophilic ability is strong. It is...

Claims

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Application Information

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IPC IPC(8): C25B3/07
CPCC25B3/00
Inventor 李美超尹文旭赵灵敏沈振陆
Owner ZHEJIANG UNIV OF TECH
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