HRID1091146

反应详情

EQUATION

反应方程式

HRID 1091146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 6 g of 5-nitro-2-hydroxy-N-(1H-indol-4-yl)-benzamide of Example 50, 600 ml of methanol and 15 ml of 64% hydrazine hydrate and 6 g of Raney nickel was refluxed for two hours and filtered. The filtrate was evaporated to dryness under pressure at 50° C. and the residue was taken up in a 1-1 mixture of chloroform and methanol. The mixture was filtered and the crystalline product was dried to obtain 4 g of 5-amino-2-hydroxy-N-(1H-indol-4-yl)-benzamide melting at >260° C.

WORKUP

后处理

  1. temperaturewas refluxed for two hours
  2. filtrationfiltered
  3. customThe filtrate was evaporated to dryness under pressure at 50° C.
  4. additionthe residue was taken up in a 1-1 mixture of chloroform and methanol
  5. filtrationThe mixture was filtered
  6. customthe crystalline product was dried