HRID442406
反应详情
EQUATION
反应方程式
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反应物
PRODUCTS
生成物
PROCEDURE
实验过程
86 g (1 mol) of methacrylic acid were added dropwise to 117 g (1 mol) of methyldichlorophosphine at a temperature from 40° to 45° C. The mixture was stirred for 1 hour at said temperature. Phosphinic-carboxylic acid dichloride was then decomposed with 18 ml of H2O at a temperature of from 40° to 60° C., whereby a considerable formation of hydrogen chloride occurred. The residual quantity of hydrogen chloride in the reaction mixture was removed in a water-jet vacuum at 150° C. The residue was distilled under reduced pressure. 126 g of 2,4-dimethyl-2,5-dioxo-1,2-oxa-phospholane were obtained, which corresponds to a yield of 85.1% of the theory.
WORKUP
后处理
- customThe residual quantity of hydrogen chloride in the reaction mixture was removed in a water-jet vacuum at 150° C
- distillationThe residue was distilled under reduced pressure