HRID2235444

反应详情

EQUATION

反应方程式

HRID 2235444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A solution of N-(3,3-dimethyl-6-nitro-2-oxo-2,3-dihydro-1H-indol-5-yl)4-methoxy-benzamide (200 mg), allyl bromide (78 mg; 0.65 mmol) and K2CO3 (233 mg; 1.69 mmol) in acetone (3.2 ml) and N,N-dimethylformamide (1.6 ml) is stirred at 50° C. for 48 h. The mixture is filtered and concentrated in vacuo. The residue is suspended in acetic acid (3 ml), iron (150 mg; powder) is added and the resulting mixture is heated in a microwave apparatus at 150° C. for 900 s. After re-cooling the mixture is filtered and concentrated in vacuo. The desired compound is obtained by preparative RP-HPLC.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. concentrationconcentrated in vacuo
  3. additioniron (150 mg; powder) is added
  4. temperatureAfter re-cooling the mixture
  5. filtrationis filtered
  6. concentrationconcentrated in vacuo