反应详情

To an ice cooled solution of 1-(5-bromo-2-fluorophenyl)-2,2-difluoropropane-1,3-diol (17.0 g, 59.8 mmol) in dry DCM (200 mL) was added imidazole (12.2 g, 179.2 mmol) at 0° C. and stirred for 15 min. tert-butyldimethylsilylchloride (13.5 g, 89.5 mmol) was added to the resultant reaction mixture portion wise for a period of 30 min. and stirring continued for 2 h. Reaction was monitored by TLC analysis. The solids formed in the reaction mixture were separated by filtration and filtrate was concentrated under reduced pressure to obtain crude product which was purified by column chromatography on silica gel with 2% Ethylacetate in Hexane as eluent to furnish title compound as a colorless liquid. Yield=19 g (80%). TLC (20% ethyl acetate in Hexane): Rf=0.75),

1. additionwas added to the resultant
2. customreaction mixture portion wise for a period of 30 min.
3. customReaction
4. customThe solids formed in the reaction mixture
5. customwere separated by filtration and filtrate
6. concentrationwas concentrated under reduced pressure
7. customto obtain crude product which
8. customwas purified by column chromatography on silica gel with 2% Ethylacetate in Hexane as eluent