反应详情

Methanesulfonyl chloride (3.68 mL, 47.6 mmol) was added dropwise as a solution in CH2Cl2 (20 mL) to a solution of Compound B (10 g, 36.6 mmol) in CH2Cl2 (130 mL) at 0° C. under argon. After stirring at rt for 16 hr the reaction was diluted with water (20 mL). The layers were separated and the aqueous layer was extracted with CH2Cl2 (2×40 mL). The combined organic layers were washed with water (1×30 mL), KHSO4 (2×30 mL), water (1×30 mL), NaHCO3 (2×30 mL), brine (1×30 mL), dried over MgSO4, filtered and concentrated to afford a golden brown oil. The oil was crystalized from EtOAc/hexanes and the yellow solid triturated with hexane and dried to afford Compound C (10.6 g, 82 %). MS: [M+H]+ =351

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with CH2Cl2 (2×40 mL)
3. washThe combined organic layers were washed with water (1×30 mL), KHSO4 (2×30 mL), water (1×30 mL), NaHCO3 (2×30 mL), brine (1×30 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto afford a golden brown oil
8. customThe oil was crystalized from EtOAc/hexanes
9. customthe yellow solid triturated with hexane
10. customdried