HRID52608

反应详情

EQUATION

反应方程式

HRID 52608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 0.5 g (0.00175 mol) of 1,4-diketo-3,6-diphenylpyrrolo[3,4-c]pyrrole in 17 ml of tetrahydrofuran are added, under argon, 0.28 g (0.007 mol) of solid sodium hydride. After stirring for 24 hours, 0.67 ml (0.007 mol) of n-butyl chloroformate are added and the suspension is stirred overnight. The mixture is filtered and the filtrate is concentrated under vacuum. The residue is taken up in water/diethyl ether, the organic phase is dried over MgSO4 and then concentrated under vacuum. The residue is taken up in n-hexane and the precipitated yellow powder is collected by filtration and washed with a minor amount of n-hexane, giving 0.62 g (73% of theory) of N,N'-bis(n-butoxycarbonyl)-1,4-diketo-3,6-diphenylpyrrolo[3,4-c]pyrrole as a yellow fluorescent powder.

WORKUP

后处理

  1. additionare added, under argon
  2. stirringthe suspension is stirred overnight
  3. filtrationThe mixture is filtered
  4. concentrationthe filtrate is concentrated under vacuum
  5. dry with materialthe organic phase is dried over MgSO4
  6. concentrationconcentrated under vacuum
  7. filtrationthe precipitated yellow powder is collected by filtration
  8. washwashed with a minor amount of n-hexane