HRID640867

反应详情

EQUATION

反应方程式

HRID 640867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A dry 50 mL flask was charged with N-[4-(3-Hydroxymethylene-2-oxo-2,3-dihydro-1H-indole-6-carbonyl)-phenyl]-acetamide (prepared below, 70 mg, 0.217 mmol) and Dioxane (10 mL). To the resulting solution was added N-(4-aminophenyl)morpholine (200 mg, 1.122 mmol), and the mixture was stirred for 24 h at 100° C. Subsequently, the reaction mixture was cooled to room temperature. The resulting suspension was concentrated in vacuo and the resulting solid residue was recrystallized from iPrOH (˜5 mL). The solid recovered through filtration then was subjected to flash silica gel chromatography using a 5% MeOH/CHCl3 eluant mixture to afford the title compound in 33% yield (35 mg, 0.072 mmol).

WORKUP

后处理

  1. temperatureSubsequently, the reaction mixture was cooled to room temperature
  2. concentrationThe resulting suspension was concentrated in vacuo
  3. customthe resulting solid residue was recrystallized from iPrOH (˜5 mL)
  4. filtrationThe solid recovered through filtration