反应详情

温度

0 °C

In 460 ml of dimethylformamide, 46.0 g (0.21 mole) of the 3-(3,4-dichlorophenyl)-3-oxo-1-propanol obtained in Referential Example 4(a) were dissolved, followed by the addition of 35 ml (0.25 mole) of triethylamine and 38.0 g (0.25 mole) of tert-butyldimethylchlorosilane under ice-cooling. The resulting mixture was stirred at 0° C. for 2 hours. The reaction mixture was poured into water and the mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give a residue, which was purified by chromatography on a silica gel column (eluting solvent: n-hexane: ethyl acetate=96:4), whereby 66.1 g of the title compound were obtained as white crystals.

1. dissolutionwere dissolved
2. temperaturecooling
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customto give a residue, which
8. customwas purified by chromatography on a silica gel column (eluting solvent: n-hexane: ethyl acetate=96:4)