反应详情

A solution of tosyl chloride (20 g, 0.1 mol) in diethyl ether (100 ml) was added in drops at room temperature to a solution of D-valine (11.7 g, 0.1 mol) in 200 ml of 1N NaOH, and the two-phase mixture was stirred vigorously for 4 hours. Then, the diethyl ether phase was separated, the aqueous phase was washed twice more with diethyl ether and acidified at 0° C. by adding concentrated HCl. After 30 minutes, it was suctioned off, liberally rewashed with ice water and dried for several hours at 0.01 Torr. 18.1 g, (67%), of colorless crystals was obtained (melting point: 147° C.).

1. customThen, the diethyl ether phase was separated
2. washthe aqueous phase was washed twice more with diethyl ether
3. customacidified at 0° C.
4. additionby adding concentrated HCl
5. waitAfter 30 minutes
6. customdried for several hours at 0.01 Torr
7. custom18.1 g, (67%), of colorless crystals was obtained (melting point: 147° C.)