HRID231166

反应详情

EQUATION

反应方程式

HRID 231166 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.3 g (4.2 mmol) of the title compound from Example 28 were dissolved in 25 ml of anhydrous pyridine, and 50 mg of 4-dimethylaminopyridine were added. Under a nitrogen atmosphere and while stirring, 6.3 ml acetic anhydride were added dropwise, and the mixture was stirred at room temperature for one hour. It was then poured onto ice water, extracted with methylene chloride, and the organic phase was dried over MgSO4 and concentrated in vacuo. The crystalline solid was recrystallized from ethanol. Melting point 111°-113° C.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for one hour
  2. additionIt was then poured onto ice water
  3. extractionextracted with methylene chloride
  4. dry with materialthe organic phase was dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe crystalline solid was recrystallized from ethanol