HRID411767

反应详情

EQUATION

反应方程式

HRID 411767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension consisting of 0.5 g (1.25 mmole) of 3-(1-methyl-3-indolyl)-4-(1-methyl-6-nitro-3-indolyl)-1H-pyrrole-2,5-dione (See Davis U.S. Pat. No. 5,057,614), 4.0 ml of formaldehyde solution (37% w/w), and 2.0 ml of water was heated to 125° C. with stirring and with a reflux condensed attached for 14 hours. The reaction mixture was cooled and diluted with water. The red solid was filtered, washed with water and dried. The solid was purified by chromatography using silica gel and a mixture of EtOAc/Hexane as elutant to afford 1-hydroxymethyl-3-(1-methyl-1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-pyrrole-2,5-dione (mp=209-211° C.).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. filtrationThe red solid was filtered
  3. washwashed with water
  4. customdried
  5. customThe solid was purified by chromatography
  6. additiona mixture of EtOAc/Hexane as elutant