HRID862373

反应详情

EQUATION

反应方程式

HRID 862373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.28 g (0.007 mol) of solid sodium hydride is added to a suspension of 0.5 g (0.00175 mol) of 1,4-diketo-2,5-dihydro-3,6-diphenyl-pyrrolo[3,4-c]pyrrole in 17 ml of tetrahydrofuran in an argon atmosphere. After the resulting mixture is stirred for 24 hours, 0.67 ml (0.007 mol) of n-butyl chloroformate is added thereto, and the resulting suspension is stirred overnight. The mixture is filtered, and the filtrate is concentrated under reduced pressure. The residue is taken into water/diethyl ether, and the organic phase is dried over MgSO4 and then concentrated under reduced pressure. The residue is taken into n-hexane, and the yellow powder precipitated is collected by filtration, washed with a small amount of n-hexane to give 0.62 g (73% of the theoretical value) of N,N'-bis(n-butoxycarbonyl)-1,4-diketo-2,5-dihydro-3,6-diphenyl-pyrrolo[3,4-c]pyrrole as a yellow fluorescent powder.

WORKUP

后处理

  1. stirringthe resulting suspension is stirred overnight
  2. filtrationThe mixture is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. dry with materialthe organic phase is dried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customthe yellow powder precipitated
  7. filtrationis collected by filtration
  8. washwashed with a small amount of n-hexane