反应详情

温度

50 °C

S-4-(3,3,3-trifluoropropanamido)phenyl 3,3,3-trifluoropropanethioate (44.8 g, 189 mmol) and EtOH (70 mL) are charged to a flask. Concentrated HCl (22.5 mL) is slowly added to keep the temp below 30° C. The reaction is then heated to 50° C. for 17.5 h. The reaction mixture is reduced to 41 mL by vacuum distillation at 50° C. Cool the reaction to room temperature and H2O (51 mL) is added. The slurry is filtered and the filter cake is washed with H2O (3×35 mL). The solid is dried under vacuum to produce the desired compound (19.9 g, 58%).

1. customthe temp below 30° C
2. distillationThe reaction mixture is reduced to 41 mL by vacuum distillation at 50° C
3. temperatureCool
4. customthe reaction to room temperature
5. filtrationThe slurry is filtered
6. washthe filter cake is washed with H2O (3×35 mL)
7. customThe solid is dried under vacuum