反应详情

Diisopropylethylamine (1.6 mL, 9.18 mmol) was added to a solution of alcohol (10) (1.2 g, 3.06 mmol 3.0 eq) in CH2Cl2 (30 mL) followed by MsCl (0.28 mL, 3.67 mmol, 1.2 eq). The solution was stirred at room temperature for 2 hours, then quenched with water and diluted with CH2Cl2 (200 mL). The organic layer was washed with brine, 1N HCl, saturated NaHCO3, and dried over MgSO4. The crude oil was purified by flash chromatography (CH2Cl2—MeOH/95:5) to give light yellow solid (1.43 g, 99.3%).

1. customquenched with water
2. additiondiluted with CH2Cl2 (200 mL)
3. washThe organic layer was washed with brine, 1N HCl, saturated NaHCO3
4. dry with materialdried over MgSO4
5. customThe crude oil was purified by flash chromatography (CH2Cl2—MeOH/95:5)