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Catalystic preparation of nitrine diphenyl posphate

A technology of diphenyl azide phosphoric acid and diphenyl chlorophosphoric acid is applied in the field of preparing diphenyl phosphoric acid azide by using phase transfer catalyst catalysis, and can solve the problem that the reactant and the target product are difficult to be separated, and the yield and purity of the target product can be solved. It is not high, the preparation reaction time is long, etc., to achieve the effect of easy large-scale industrial preparation, short time and simple operation

Inactive Publication Date: 2004-12-08
GUILIN GUIKAI BIOLOGICAL SCI & TECH
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  • Description
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Problems solved by technology

[0005] The above two methods all have defects such as long preparation reaction time, complicated operation, difficult separation of reactants and target products, and low yield and purity of target products.

Method used

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  • Catalystic preparation of nitrine diphenyl posphate
  • Catalystic preparation of nitrine diphenyl posphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 47.9g (0.178mol) of diphenyl chlorophosphate, 20.7g (0.32mol) of sodium azide, and 2.5g of tetrabutylammonium bromide into a 100ml three-necked flask and stir vigorously at room temperature for 10 hours. Viscous, then gradually become thinner, the color changes from colorless to light gray, and can be filtered to obtain 42.5g of slightly light yellow or colorless slightly viscous liquid, the yield is 86.2%, and the HPLC content is 99.3%.

[0021] Analysis data: IR(cm -1 ) 3060 (w, C-H), 2170 (s, -N3), 1590 (m), 1490 (s, C=C), 1270 (m, P=O), 960 (s, P-O-Aryl).

Embodiment 2

[0023] Add 48.1g (0.18mol) of diphenyl chlorophosphate, 27.6g (0.42mol) of sodium azide, and 3.0g of TEBA into a 100ml three-neck flask, stir vigorously at room temperature for 15 hours, and filter to obtain 41.8g of slightly light yellow liquid , HPLC content 97.7%, yield 85.2%.

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Abstract

A process for preparing diphenyl azidophosphate by catalytic method features the reaction between its raw materials (diphenyl chlorophosphate and sodium azide) and the phase-transfer catalyst chosen from quaternary ammonium salt, inorganic tetraamine salt, strong-alkaline alamine and crown ether at 15-30 deg.c for 10-15 hr. Its advantages are simple process and high purity of product.

Description

technical field [0001] The invention relates to a preparation method of diphenyl phosphoric azide, in particular to a method for preparing diphenyl phosphoric azide as catalyzed by a phase transfer catalyst. technical background [0002] Diphenylphosphoryl azide (DPPA for short) is a widely used organophosphorus reagent in organic synthesis, and its chemical structural formula is as follows: [0003] [0004] The existing preparation method of diphenylphosphoric azide is mainly divided into two kinds, one is the solvent method, that is, diphenyl chlorophosphoric acid is used as raw material, and anhydrous acetone is used as solvent to react with sodium azide to obtain azide Nitrophosphoric acid diphenyl ester (JP805459); The other is a solvent-free method, that is, at normal temperature, chlorophosphoric acid diphenyl ester and sodium azide react under solvent-free conditions to obtain the target compound ("Chemical Reagent" 1992, 14 (6) 377). [0005] The above two met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
Inventor 吴范宏辛水波
Owner GUILIN GUIKAI BIOLOGICAL SCI & TECH
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