HRID1276884

反应详情

EQUATION

反应方程式

HRID 1276884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

N-benzenesulfonyl-4-acetylamino-3-nitrobenzamide (12.67 g) was dissolved in 200 ml of methanol and 30 ml of water, and 7.59 g of potassium hydrogencarbonate were further added thereto. The mixture was hydrogenated in a hydrogen atmosphere using 2.53 g of 5% palladium on carbon as catalyst at 40° C. for 24 hours. The solid material was separated through filtration, and the filtrate was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of ethyl acetate and methanol at a ratio of 4:1) to give 6.72 g of N-benzenesulfonyl-4-acetylamino-3-aminobenzamide.

WORKUP

后处理

  1. customat 40° C.
  2. customfor 24 hours
  3. customThe solid material was separated through filtration
  4. concentrationthe filtrate was concentrated
  5. customThe resulting residue was purified through silica-gel column chromatography (eluent
  6. additiona mixture of ethyl acetate and methanol at a ratio of 4:1)