HRID394479

反应详情

EQUATION

反应方程式

HRID 394479 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Compound 6 (1.92 g, 5.26 mmol), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (4.78 g, 21.0 mmol), and acetonitrile (30 mL) were combined under argon and heated at 90° C. for 1 h. The solution was cooled and the solvent was removed in vacuo. The crude product was purified by flash column chromatography (methylene chloride:methanol:ammonium hydroxide 95:5:0.5) to give a solid. Trituration with.Et2O EtOAc gave Compound 69: 1.60 g (4.4 mmol, 83%)

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. customthe solvent was removed in vacuo
  3. customThe crude product was purified by flash column chromatography (methylene chloride:methanol:ammonium hydroxide 95:5:0.5)
  4. customto give a solid