反应详情

A solution of (S)-2-(7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-hydroxyethyl pivalate (5I) (0.016 g, 0.040 mmol) and perchloric acid, 70% (6 μl, 0.1 mmol) in tert-butyl acetate (1 mL) was stirred at room temperature for 2 h. Reaction mixture was quenched with solid sodium bicarbonate (0.05 g) for 1 h. Saturated sodium bicarbonate solution was added and extracted with ethyl acetate (3×). The combined organic layer was dried (MgSO4), concentrated and purified by flash column chromatography (silica gel, 0 to 50% ethyl acetate/hexanes). LCMS-ESI+: calc'd for C25H30ClNO3S: 460.2 (M+H+). Found: 460.2 (M+H+).

1. customReaction mixture
2. customwas quenched with solid sodium bicarbonate (0.05 g) for 1 h
3. additionSaturated sodium bicarbonate solution was added
4. extractionextracted with ethyl acetate (3×)
5. dry with materialThe combined organic layer was dried (MgSO4)
6. concentrationconcentrated
7. custompurified by flash column chromatography (silica gel, 0 to 50% ethyl acetate/hexanes)