HRID1165895

反应详情

EQUATION

反应方程式

HRID 1165895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The well-dried compound (18) (2.1 g) was dissolved in benzene (150 ml), and then trichloroacetic acid (0.4 g) was added. The mixture was heated under reflux for 2 hours on an oil bath. The reaction mixture was cooled to room temperature, and then passed through a column of alumina. From the eluted solution the solvent was distilled off to obtain the crude product (19), at a yield of 1.02 g. The crude product was purified on an alumina (20 g) column, eluting with hexane, to obtain the product (19) at a yield of 725 mg (91.2%) as a blue oily substance.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hours on an oil bath
  3. distillationFrom the eluted solution the solvent was distilled off
  4. customto obtain the crude product (19)
  5. customThe crude product was purified on an alumina (20 g) column
  6. washeluting with hexane