反应详情

温度

20 °C

To a solution of 7 g (37.8 mmol) of (1-amino-2-phenylethyl)phosphinic acid in 86 ml of a mixture of dioxane and water, in the presence of one equivalent of sodium hydroxide (1.51 g), are added dropwise, at 0° C and simultaneously, a solution of 7.55 g (44.26 mmol) of benzyl chloroformate in 21 ml of dioxane and, in order to keep the pH of the reaction at about 9, a solution of 2.42 g of sodium hydroxide in 21 ml of water. At the end of the addition, the mixture is maintained at a temperature in the region of 20° C. for 2 hours. The aqueous phase is then washed with 3 times 20 ml of diethyl ether. The aqueous phase is acidified, at 0° C., with vigorous stirring, using 27 ml of 6N hydrochloric acid solution. The abundant white precipitate formed is filtered off, washed with water and dried. 12.08 g of product are recovered (yield=83.7%).

1. customthe pH of the reaction at about 9
2. additionAt the end of the addition
3. washThe aqueous phase is then washed with 3 times 20 ml of diethyl ether
4. customis acidified, at 0° C., with vigorous stirring
5. customThe abundant white precipitate formed
6. filtrationis filtered off
7. washwashed with water
8. customdried
9. custom12.08 g of product are recovered (yield=83.7%)