Method for continuously and rapidly preparing N-phenylthiophosphoryl dichloride by utilizing micro-reactor

A kind of phenyl thiophosphoryl dichloride and microreactor technology, which is applied in the field of synthesizing N-phenyl thiophosphoryl dichloride

Inactive Publication Date: 2020-10-23
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In a microreactor, synthesized from phosphorus trichloride and aniline N -The method of phenylphosphoryl dichloride has not been reported yet

Method used

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  • Method for continuously and rapidly preparing N-phenylthiophosphoryl dichloride by utilizing micro-reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] As shown in the figure, the tetrahydrofuran solution of phosphorus trichloride R1 (0.1 mol / L) and aniline R2 (0.2 mol / L) was injected into the micro-mixer B1 (T -type tee, inner diameter: 1 mm) after mixing, enter the microchannel reactor C1 (inner diameter: 1 mm) and continue in the low temperature tank D1 (-20 o In C), the nucleophilic addition was carried out and reacted for 60 min. The sample was collected with the product collection bottle E, and the HCl was treated with the gas absorption bottle F and then emptied. The crude product is separated, purified and refined to obtain N -Phenylphosphoryl dichloride. Product GC analysis yield 67%, selectivity 90%.

Embodiment 2

[0017] As shown in the figure, the 1,4-dioxane solution of phosphorus trichloride R1 (0.5 mol / L) and aniline R2 (1.0 mol / L) is respectively supplied by high-pressure syringe pumps A1 and A2 according to the molar ratio of 1:1 After being injected into the micro-mixer B1 (Y-type micro-mixer, inner diameter: 3 mm) for mixing, it enters the microchannel reactor C1 (inner diameter: 3 mm) and continues in the low-temperature tank D1 (-10 o In C), carry out nucleophilic addition and react for 30 min, the sample is collected with the product collection bottle E, and the HCl is treated with the gas absorption bottle F and then emptied. The crude product is separated, purified and refined to obtain N -Phenylphosphoryl dichloride. Product GC analysis yield 80%, selectivity 91%.

Embodiment 3

[0019] As shown in the figure, the benzene solutions of phosphorus trichloride R1 (0.5 mol / L) and aniline R2 (1.5 mol / L) were injected into the micro-mixer B1 (J -type micro-mixer, inner diameter: 6 mm) after mixing, enter the microchannel reactor C1 (inner diameter: 3 mm) and continue in the low-temperature tank D1 (0 o In C), the nucleophilic addition was carried out and reacted for 40 min. The sample was collected with the product collection bottle E, and the HCl was treated with the gas absorption bottle F and then emptied. The crude product is separated, purified and refined to obtain N -Phenylphosphoryl dichloride. Product GC analysis yield 84%, selectivity 94%.

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Abstract

The invention discloses a method for continuously and rapidly preparing N-phenylthiophosphoryl dichloride by utilizing a micro-reactor. In a microstructure reactor, thiophosphoryl chloride and anilineare used as raw materials, and a nucleophilic addition reaction is carried out under a continuous flow condition; and a crude product is subjected to separating and purifying to obtain the high-quality N-phenylthiophosphoryl dichloride. The method has the characteristics of rapid and continuous preparation of N-phenylthiophosphoryl dichloride, simple operation, continuous and controllable process, mild conditions, good product selectivity, and capacity of realizing industrial production.

Description

technical field [0001] The invention relates to a rapid, continuous and highly selective synthesis in a microreactor N - The method of phenylphosphoryl dichloride. Background technique [0002] N -Phenylphosphoryl dichloride is an important intermediate used in the synthesis of medicines, biological products and fine chemicals, especially for the preparation of oligonucleotide phosphorodithioate, which has attracted much attention. [0003] Piotto et al. (M. E. Piotto, J. N. Granger, Y. Cho, N. Farschtschi, D. G. Gorenstein. Tetrahedron , 1991, 47, 2449-24611.) Using phosphorus trichloride, aniline, benzene, and 20% aqueous sodium hydroxide as raw materials, under low temperature conditions (-5 o C) The reaction produces a N - Suspension of phenylphosphoryl dichloride, diluted with benzene, washed with saturated NaCl solution containing 1% sodium bisulfate, and then prepared through a series of post-treatments N -Phenylphosphorylthiodichloride, the yield is 72.0%. The ...

Claims

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Application Information

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IPC IPC(8): C07F9/26
CPCC07F9/26
Inventor 邓秋林雷琴廖辉伟黄晓枫
Owner SOUTHWEAT UNIV OF SCI & TECH
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