反应详情

A mixture of 2-(3,4-dichloro-phenylamino)-propionic acid ethyl ester (10.0 g, 38.1 mmol) and LiOH (2.74 g, 114 mmol) in THF/MeOH/water 2:1:1 (100 mL) was heated at reflux for 3 h, then after cooling poured onto water and extracted with TBME. The organic phase was extracted twice with 1 M aq. sodium hydroxide solution. The aqueous phases were combined, acidified to pH 2-3 by addition of 37% aq. HCl solution, and extracted with EtOAc. The organic layer was dried (MgSO4), filtered, and evaporated to produce the title compound (7.32 g, 82%). Light yellow solid, MS: 233.9 (M+H)+.

1. temperaturewas heated
2. temperatureat reflux for 3 h
3. temperatureafter cooling
4. additionpoured onto water
5. extractionextracted with TBME
6. extractionThe organic phase was extracted twice with 1 M aq. sodium hydroxide solution
7. additionacidified to pH 2-3 by addition of 37% aq. HCl solution
8. extractionextracted with EtOAc
9. dry with materialThe organic layer was dried (MgSO4)
10. filtrationfiltered
11. customevaporated