Benzyl chloroformate → HCID 178465414, compound

Temperature

20 °C

To a solution of 1.7 g (15.6 mmol) of 1-aminoethyl phosphinic acid in 35 ml of a mixture of dioxane and water, in the presence of an equivalent of soda (624 mg), there is added, 0° C., dropwise and simultaneously, a solution of 3.1 g (18.3 mmol) of benzyl chloroformate in 9 ml of dioxane and, so as to maintain the pH of the reaction about 9, a solution of 1 g of soda in 8.7 ml of water. At the end of the addition, the mixture is maintained at a temperature about 20° C. for 2 hours. The aqueous phase is then washed 3 times with 20 ml of diethyl ether. The aqueous phase is acidified, at 0° C., with brisk agitation, with 11 ml of a 6N hydrochloric acid solution. An abundant white precipitate forms, which is filtered, washed with water and dried. There is recovered 2.8 g of product (yield=73.9%).

1. customthe pH of the reaction about 9
2. additionAt the end of the addition
3. washThe aqueous phase is then washed 3 times with 20 ml of diethyl ether
4. customis acidified, at 0° C., with brisk agitation, with 11 ml of a 6N hydrochloric acid solution
5. filtrationAn abundant white precipitate forms, which is filtered
6. washwashed with water
7. customdried

ORD record

ord-ddedc22613d148eda6d821f8dac8e4b8

Source dataset

uspto-grants-2002_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06391866B1