HRID21532

反应详情

EQUATION

反应方程式

HRID 21532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound of Example 2 (988 mg, 5.0 mmol) was dissolved in 30 ml of anhydrous pyridine. After addition of 0.6 ml (5.5 mmol) of isopropenyl chloroformate, the mixture was stirred at room temperature for 4 h and subsequently concentrated. The residue was dissolved in ethyl acetate and washed three times with water, dried (sodium sulfate) and concentrated. After chromatography on silica gel (ethyl acetate/heptane=1:2), the desired compound was isolated and crystallized from diethyl ether/pentane; yield 380 mg (27%) of melting point 86°-87° C.

WORKUP

后处理

  1. concentrationsubsequently concentrated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed three times with water
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated