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) were charged to a flask. Concentrated HCl (22.5 mL) was slowly added to keep the temperature below 30° C. The reaction was then heated to 50° C. for 17.5 h. The reaction mixture was reduced to 41 mL by vacuum distillation at 50° C. Cool the reaction to room temperature and H2O (51 mL) was added. The slurry was filtered and the filter cake was washed with H2O (3×35 mL). The solid was dried under vacuum to produce the desired compound (19.9 g, 58%).

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