HRID973613
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 2.7 g of ethyl trimethylsilyldiethoxymethylphosphonite and 0.7 g of methyl vinyl ketone is warmed to 50° for 1 hour under an atmosphere of nitrogen. Then 10 ml of water are added and the mixture is stirred for additional 30 minutes. The residue is extracted thrice with 50 ml of chloroform, the organic phases are combined, dried over magnesium sulphate, filtered and evaporated to dryness. The residue is then distilled to yield ethyl 3-oxobutyl(diethoxymethyl)phosphinate, b.p. 130°-5° (13.6 mbar).
WORKUP
后处理
- temperatureis warmed to 50° for 1 hour under an atmosphere of nitrogen
- extractionThe residue is extracted thrice with 50 ml of chloroform
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customevaporated to dryness
- distillationThe residue is then distilled