反应详情

1.15 g of 3-amino-3-phenylpropionic acid are dissolved in 25 ml of dioxane and 7 ml of 1N sodium hydroxide and 1.95 g of 2,4,6-trichlorobenzenesulphonyl chloride in 5 ml of dioxane are gradually added, while maintaining the pH at 10.5-11 by addition of 1N sodium hydroxide. After stirring for 2 hours at RT, the mixture is diluted with 100 ml of water, extracted twice with EtOAc and acidified to pH=2 by addition of 6N HCl. The solid formed is drained, washed with water and dried at 40° C. 2.09 g of the expected product are obtained, m.p.−218-219° C.

1. temperaturewhile maintaining the pH at 10.5-11
2. extractionextracted twice with EtOAc
3. additionacidified to pH=2 by addition of 6N HCl
4. customThe solid formed
5. washwashed with water
6. customdried at 40° C