反应详情

To a solution of 1 g (3.13 mmol) of [2-phenyl-1-[[(phenylmethoxy)carbonyl]amino]ethyl]phosphinic acid synthesized in 1.4., 2.2 g (14.10 mmol) of ethyl 4-methyl-2-methylenepentanoate and 0.52 ml of N,O-bis(trimethylsilyl)acetamide in 0.27 ml of acetonitrile is stirred at a temperature in the region of 20° C. for 24 hours. 60 ml of a 1/1 ethyl acetate/water mixture are added. The aqueous phase is extracted with ethyl acetate and the combined organic phases are washed with water, dried over sodium sulphate, filtered and evaporated under vacuum. The product is purified by recrystallization from a mixture of ethyl acetate and hexane. 1.21 g of product are recovered (yield=81.3%).

1. extractionThe aqueous phase is extracted with ethyl acetate
2. washthe combined organic phases are washed with water
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customevaporated under vacuum
6. customThe product is purified by recrystallization from a mixture of ethyl acetate and hexane
7. custom1.21 g of product are recovered (yield=81.3%)