HRID1582650

反应详情

EQUATION

反应方程式

HRID 1582650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-(3,4-Dichlorobenzyl)-5-hydroxyindole-2-carboxylic acid (10 g) in warm ethyl acetate (250 ml) was added 4-dimethylaminopyridine (100 mg) and acetic anhydride (5.0 ml) and the resulting mixture was stirred for 2 hours. The organics were washed with 1N HCl and dried. Hexane was added to cause crystallision of the product. The solid was filtered and washed with hexane to give the desired product. (5 g, 44%). 1H NMR (DMSO-d6) δ 2.25 (s, 3H), 5.85 (s, 2H), 6.9 (dd, 1H), 7.05 (dd, 1H), 7.3-7.6 (m, 5H); m/z 378, 380 (MH+).

WORKUP

后处理

  1. washThe organics were washed with 1N HCl
  2. customdried
  3. additionHexane was added
  4. customcrystallision of the product
  5. filtrationThe solid was filtered
  6. washwashed with hexane