反应详情

To a 100 ml round bottom flask was loaded 4-(trifluoromethoxy)benzoic acid (4.85 g, 23.5 mmol). Thionyl chloride (5.15 ml, 70.6 mmol) was added at 0° C. The reaction mixture was allowed to warm up to room temperature and then heated at 80° C. for 1 hour. After cooling down to room temperature, the volatiles were removed. The residue was diluted with 50 ml methylene chloride, and 2-amino-2-methylpropan-1-ol (7.34 g, 82 mmol) was added at 0° C. The reaction mixture was allowed to warm up to room temperature. It was diluted with 150 ml ether, washed sequentially with 100 ml 1N HCl, 100 ml 5% KOH and 50 ml brine. The organics were dried over sodium sulfate, filtered and concentrated to give 4.2 g desired product. It was used for the next step directly without further purification.

1. customTo a 100 ml round bottom flask was loaded
2. temperatureheated at 80° C. for 1 hour
3. temperatureAfter cooling down to room temperature
4. customthe volatiles were removed
5. additionwas added at 0° C
6. temperatureto warm up to room temperature
7. washwashed sequentially with 100 ml 1N HCl, 100 ml 5% KOH and 50 ml brine
8. dry with materialThe organics were dried over sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated