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Preparation method of phosphous dihalide with substituent group

A technology of phosphorus dihalide and phosphoryl phosphorus trihalide, which is applied in chemical instruments and methods, organic chemistry, and compounds of Group 5/15 elements of the periodic table, etc., which can solve the difficulties of product separation and purification, unstable process routes, and equipment Harsh requirements and other issues, to achieve the effect of high reaction yield, easy industrial implementation, and no three wastes

Inactive Publication Date: 2006-05-03
SHANGHAI UNIV OF ENG SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to disclose a new preparation method of phosphorus dihalides with substituents, so as to overcome the low total yield, harsh equipment requirements, unstable process route, and difficulty in product separation and purification in the prior art. defect

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  • Preparation method of phosphous dihalide with substituent group

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Embodiment 1

[0028] Add 412 grams of phosphorus trichloride and 515 grams of tetraphenyl lead successively in a nitrogen-dried reaction flask equipped with mechanical stirring, a constant pressure dropping funnel, and a thermometer. Vigorously stirred at 180°C, a gray precipitate was produced as the reaction progressed, and the reaction was stopped after stirring for 180 hours. Directly carry out vacuum distillation to obtain 500 grams of phenylphosphorous dichloride, the yield is 93%, 31 P NMR (CDCl 3 , 100MHz): -161.8ppm

Embodiment 2

[0030] Add 731 grams of phosphorus tribromide successively in a nitrogen-dried reaction flask equipped with mechanical stirring, a constant pressure dropping funnel, and a thermometer, and then add 323 grams of tetraethyl lead dropwise to the reaction system. During the dropwise addition, Accompanied by a violent exotherm. Vigorously stirred at 20°C, a gray precipitate was produced as the reaction progressed, and the reaction was stopped after stirring for 35 hours. Directly carry out vacuum distillation to obtain 356 grams of ethyl phosphorus dibromide, and the yield is 60%, 31 P NMR (CDCl 3 , 100MHz): -194.8ppm.

Embodiment 3

[0032] Add 458 grams of sulfuryl phosphorus trichloride successively in a nitrogen-dried reaction flask equipped with mechanical stirring, a constant pressure dropping funnel, and a thermometer, and then slowly add 323 grams of tetraethyl lead dropwise to the reaction system. After the dropwise addition, stir vigorously at 20°C for one hour, then gradually raise the temperature to 70°C, and continue to stir for 45 hours. As the reaction proceeds, gray precipitates are formed. After continuing to stir for 19 hours, stop the reaction. Directly carry out vacuum distillation to obtain 402 grams of sulfuryl ethyl phosphorus dichloride. (Yield: 90%) 31 P NMR (CDCl 3 , 100MHz): -94.3ppm.

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Abstract

The invention discloses a preparation method for phosphous dihalide with substituent, which comprises: using phosphous trihalide, phosphoryl phosphous trihalide or sulphuryl group to react with a metal tetra-alkyl, tetraene or tetra-aryl compound for 0.5~300h at 0~350Deg regardless the catalyst and solvent. This invention needs mild condition, and has high yield.

Description

technical field [0001] The invention relates to a method for preparing phosphorus dihalides with substituents, in particular to a method for preparing aryl, alkenyl, alkyl phosphorus dihalides or aryl, alkenyl, alkyl substituted acyl, sulfuryl phosphorus dihalides. Background technique [0002] The phosphorus dihalides with substituents referred to in the present invention are various aryl, alkenyl, alkyl phosphorus dihalides or various aryl, alkenyl, alkyl substituted acyl, sulfuryl phosphorus dihalides, which have The phosphorus dihalide of the substituent is an important intermediate, which is widely used in fine chemical products such as pesticides and medicines. [0003] Many patents and documents disclose respective preparation methods, such as: CA: 64,2128c (1966); CA: 57,16660e (1962), all described in detail the preparation method of the phosphorus dihalide having substituent However, the technologies disclosed in the mentioned patents and documents all have proble...

Claims

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Application Information

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IPC IPC(8): C07F9/52
Inventor 严政军陈思浩徐菁利
Owner SHANGHAI UNIV OF ENG SCI
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