反应详情

To a suspension of Intermediate 20 (0.04 g, 0.192 mmol) in ethanol (2.5 mL), 4-(trifluoromethyl)aniline (ALDRICH, 0.031 g, 0.192 mmol) was added and the mixture was stirred under reflux for 2 h. Solvent was removed in vacuo and the crude mixture was purified by preparative HPLC (SunFire 19×150 mm, H2O 0.1% TFA-ACN 0.1% TFA gradient from 10 to 100%) to yield a beige solid which was further purified by preparative HPLC (SunFire 19×150 mm, H2O 0.1% TFA-ACN 0.1% TFA gradient from 30 to 100%) to yield the title compound as a white solid.

1. additionwas added
2. temperatureunder reflux for 2 h
3. customSolvent was removed in vacuo
4. customthe crude mixture was purified by preparative HPLC (SunFire 19×150 mm, H2O 0.1% TFA-ACN 0.1% TFA gradient from 10 to 100%)
5. customto yield a beige solid which
6. customwas further purified by preparative HPLC (SunFire 19×150 mm, H2O 0.1% TFA-ACN 0.1% TFA gradient from 30 to 100%)