反应详情

To a 0° C. solution of 2-[(4-amino)phenyl]ethanol (25 g), diisopropylethylamine (23.9 g) and dichloromethane (400 mL) was added heptafluorobutyryl chloride (41.8 g) dropwise over 0.5 hour. The mixture was allowed to warm gradually to room temperature and stirred for 2 hours. The precipitate was filtered off and the filtrate was diluted with ethylacetate (100 mL), washed with water (3×500 mL), dried over sodium sulfate, filtered and concentrated with a rotary evaporator. The residue was triturated with dichloromethane and collected by filtration. The combined solids were dissolved in diethyl ether and washed with water and saturated aqueous sodium chloride solutions, dried over sodium sulfate, filtered and concentrated to give 2,2,3,3,4,4,4-heptafluoro-N-[4-(2-hydroxyethyl)phenyl]butanamide as a white solid (39.2 g).

1. filtrationThe precipitate was filtered off
2. additionthe filtrate was diluted with ethylacetate (100 mL)
3. washwashed with water (3×500 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated with a rotary evaporator
7. customThe residue was triturated with dichloromethane
8. filtrationcollected by filtration
9. dissolutionThe combined solids were dissolved in diethyl ether
10. washwashed with water and saturated aqueous sodium chloride solutions
11. dry with materialdried over sodium sulfate
12. filtrationfiltered
13. concentrationconcentrated