HRID1649354
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 5.0 g (20.7 mmol) dimethyl 2,5-dimethylbenzoylphosphonate and 2.73 g (24.8 mmol) dimethyl phosphite was heated at 110° for 5 h. The excess of dimethyl phosphite and the unreacted benzoylphosphonate were removed under vacuum. The yellow viscous residue was then purified by column chromatography with chloroform as the eluent. Dimethyl α-(dimethoxyphosphinyl)2,5-dimethylbenzyl phosphate was obtained as a white oil (2.06 g, 29%); GLC and TLC analysis showed the compound to be pure.
WORKUP
后处理
- temperaturewas heated at 110° for 5 h
- customThe excess of dimethyl phosphite and the unreacted benzoylphosphonate were removed under vacuum
- customThe yellow viscous residue was then purified by column chromatography with chloroform as the eluent