反应详情

温度

10 °C

Triethylamine (20 mL, 144.6 mmol) was added to a solution of compound 54 (29.5 g, 119.9 mmol) in ethyl acetate (300 mL). The mixture was cooled to 10° C. in an ice bath. Then, a solution of mesyl chloride (10.2 mL, 131.8 mmol) in ethyl acetate (50 mL) was added dropwise at a temperature ≦20° C. The resulting solution was stirred at room temperature for 3 h (TLC monitoring, eluent: hexane-ethyl acetate, 4:1). The reaction mixture was filtered to remove the precipitate-triethylamine hydrochloride. The filtrate was washed with aqueous NaHCO3, water, and evaporated. Yield of 55: 32.2 g (83%) as crystals.

1. filtrationThe reaction mixture was filtered
2. customto remove the precipitate-triethylamine hydrochloride
3. washThe filtrate was washed with aqueous NaHCO3, water
4. customevaporated