HRID280040

反应详情

EQUATION

反应方程式

HRID 280040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customA solution formed after several minutes
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. extractionThe solution was then extracted with 0.1N HCl, 1M sodium bicarbonate, and water
  5. dry with materialdried (MgSO4)
  6. customPrecipitation with hexanes