HRID868315

反应详情

EQUATION

反应方程式

HRID 868315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Three hundred milligrams of the compound (VII) obtained in the above procedure (1) were dissolved in 80% trifluoroacetic acid solution and the resulting mixture was stirred at room temperature for 2 hours under a nitrogen gas stream. The reaction mixture was concentrated to dryness and the residue was purified by column chromatography on silica gel (10 g). A colorless oily substance was obtained from a 98:2 eluate of chloroform and methanol. The oily substance was crystallized from a mixed solvent of ethanol and petroleum ether to obtain 170 mg of the title compound as colorless needle-like crystals.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customthe residue was purified by column chromatography on silica gel (10 g)
  3. customA colorless oily substance was obtained from a 98:2 eluate of chloroform and methanol
  4. customThe oily substance was crystallized from a mixed solvent of ethanol and petroleum ether