反应详情

To a stirred solution of 4-{[tert-butyl(dimethyl)silyl]oxy}-2-chlorobenzaldehyde (WO 2003051797, 1.58 g, 5.83 mmol) in methanol (5 mL) was added sodium borohydride (264 mg, 7.00 mmol) at 0° C. The mixture was stirred at room temperature for 3 h, and quenched by addition of aqueous ammonium chloride. The mixture was extracted with ethyl acetate (200 mL), and the organic layer was washed with brine, dried over sodium sulfate, and evaporated. The residue was purified by column chromatography on silica gel (100 g) eluting with hexane/ethyl acetate (20/1 to 10/1) to afford 1.51 g (95%) of the title compound as a colorless oil:

1. customquenched by addition of aqueous ammonium chloride
2. extractionThe mixture was extracted with ethyl acetate (200 mL)
3. washthe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customThe residue was purified by column chromatography on silica gel (100 g)
7. washeluting with hexane/ethyl acetate (20/1 to 10/1)