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Method for the manufacture of dialkylphosphites

A technology of dialkyl phosphite and acid ester, applied in the field of preparing dialkyl phosphite, can solve the problems of heavy, unsuitable for commercial needs, time-consuming and the like

Inactive Publication Date: 2012-05-09
STRAITMARK HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing technologies are often onerous, time-consuming, uneconomical and ill-adapted to actual and foreseeable business needs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 22 g (0.1 mol) of P heated at 40°C 4 o 6 106 g (1.2 mol) of 1-pentanol were added dropwise with stirring over 25 minutes. The reaction mixture was maintained at 40°C while 52.56 g (0.4 mol) of 1-pentyl acetate were added. 60 ml of dry toluene was added to the reaction mixture and heating was carried out under stirring, raising the temperature to 122-135° C. to distill the toluene-rich liquid. This distillation step was maintained for 2 hours and 50 minutes with two additional additions of 60 mL of dry toluene.

[0034] crude reaction mixture 31 P NMR analysis indicated the presence of 0.5 % w / w (1.2 mol%) H 3 PO 3 , 19.6% w / w (26.1 mol%) mono-1-pentyl phosphite and 79.8% w / w (72.6 mol%) di-1-pentyl phosphite.

Embodiment 2

[0036] 22 g (0.1 mol) of P heated at 40°C 4 o 6 106 g (1.2 mol) of 1-pentanol were added dropwise with stirring over 25 minutes. While maintaining the reaction mixture at 40-50°C, 52.56 g (0.4 mol) of 1-pentyl acetate and 10 mL of 1-pentanol were added. A portion of 60 mL of dry toluene was then added to the reaction mixture and heating was applied with stirring to 120-135 °C to distill the toluene-rich liquid. After 45 minutes of distillation, 60 mL of dry toluene and 60 mL of 1-pentyl acetate were added to the reaction mixture and the heating / distillation step was further continued. This distillation step was then maintained for 4 hours and 30 minutes with the addition of 4 additional 60 mL portions of dry toluene.

[0037] in CDCl 3 crude reaction in 31 P NMR analysis indicated the presence of 0.6 % w / w (1.5 mol%) H 3 PO 3 , 19.6 % w / w (26.0 mol%) mono-1-pentyl phosphite and 79.6 % w / w (72.4 mol%) di-1-pentyl phosphite.

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Abstract

A method for the manufacture of dialkyl phosphites is disclosed wherein a P-O component containing from 1 to 6 P-O-P bonds in the molecule is reacted with an alcohol and a carboxylic acid ester having from 1 to 6 carbon atoms in the alkyl group and from 5 to 20 carbon atoms in the esterifying alkyl group of the ester. The dialkyl phosphites are formed under simultaneous removal by distillation of the carboxylic acid formed.

Description

technical field [0001] The present invention relates to a process for the preparation of dialkyl phosphite starting from a P-O component containing 1-6 P-O-P bonds in the molecule, comprising the following steps: Molar ratio, so that the P-O component and the alcohol R'OH and C 1-6 The ester of the carboxylic acid is reacted so that the esterified alkyl group contains 5-20 carbon atoms. The mixture is reacted, whereby the carboxylic acid formed is simultaneously distilled off. This process actually converts the P-O reactant very well to dialkyl phosphite with very low levels of unwanted by-products and high selectivity. In a preferred embodiment, the P-O reactant can be obtained from liquid P 4 o 6 express. Background technique [0002] Dialkyl phosphites have been known for a long time, and accordingly their importance as intermediates for the synthesis of the desired compounds has been confirmed therein. A large number of methods for the synthesis of dialkyl phosphit...

Claims

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Application Information

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IPC IPC(8): C07F9/141
CPCC07F9/1411
Inventor 帕特里克·诺特阿尔贝特·德沃
Owner STRAITMARK HLDG
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