反应详情

The compound (1.76 g) obtained in step 1 was dissolved in DMSO (30 mL), sodium hydride (0.59 g) was added at 0° C., and the mixture was stirred for 5 min. To the reaction mixture was added 2-bromo-1-chloroethane (0.77 mL), and the mixture was stirred at room temperature for 45 min. The reaction mixture was poured into water, and extracted twice with ethyl acetate. The extract was washed with saturated aqueous ammonium chloride solution, dried and concentrated under reduced pressure. The residue was separated and purified by silica gel column chromatography (10% ethyl acetate/hexane) to give methyl 1-[3,5-bis(trifluoromethyl)phenyl]cyclopropanecarboxylate (1.80 g, 94%).

1. stirringthe mixture was stirred at room temperature for 45 min
2. extractionextracted twice with ethyl acetate
3. washThe extract was washed with saturated aqueous ammonium chloride solution
4. customdried
5. concentrationconcentrated under reduced pressure
6. customThe residue was separated
7. custompurified by silica gel column chromatography (10% ethyl acetate/hexane)