HRID280040
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Compound 2 (4.10 g, 15.7 mmol) was suspended in a mixture of distilled pyridine (40 ml) and acetic anhydride (5 ml). A solution formed after several minutes, and stirring was continued overnight. The solvent was evaporated, and the residue was dissolved in ethyl acetate. The solution was then extracted with 0.1N HCl, 1M sodium bicarbonate, and water and dried (MgSO4). Precipitation with hexanes gave 3.57 g (85.1%) of a solid melting at 113°-117° C. Recrystallization from ethyl acetate/hexanes gave 2.75 g, mp 118°-120° C., [α]D25 =+15.1° (c=2.1, ethanol).
WORKUP
后处理
- customA solution formed after several minutes
- customThe solvent was evaporated
- dissolutionthe residue was dissolved in ethyl acetate
- extractionThe solution was then extracted with 0.1N HCl, 1M sodium bicarbonate, and water
- dry with materialdried (MgSO4)
- customPrecipitation with hexanes