反应详情

Chloroform (6.7 g, 2.0 eq.) was added dropwise to a stirred mixture of Ca(OH)2 (8.95 g, 120 mmol.), K2CO3 (13.5 g, 98 mmol.), 2-chloro-3-(trifluoromethyl)phenol (5.0 g, 22 mmol.), and H2O (50 mL) at 60-70° C. over 2 h. The reaction mixture was cooled, and acidified with conc. HCl. The product was extracted into EtOAc and dried over Na2SO4. Solvent was evaporated, the crude product was separated and purified through a silica column, eluting with hexane and EtOAc (3:2) to give 580 mg (10%) of the title compound.

1. temperatureThe reaction mixture was cooled
2. extractionThe product was extracted into EtOAc
3. dry with materialdried over Na2SO4
4. customSolvent was evaporated
5. customthe crude product was separated
6. custompurified through a silica column
7. washeluting with hexane and EtOAc (3:2)