HRID276023

反应详情

EQUATION

反应方程式

HRID 276023 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N,N′-carbonyldiimidazole (14.45 g) was added to a solution of 10.00 g of 4-acetylamino-3-nitrobenzoic acid in 300 ml of N,N-dimethylformamide, and the mixture was stirred at room temperature for 1 hour. Subsequently, 14.03 g of benzenesulfonamide and 13.58 g of diazabicycloundecene were added thereto, and the mixture was stirred at 100° C. for 72 hours. The reaction mixture was separated with the addition of chloroform and water. The organic layer was then concentrated, and 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 12.67 g of N-benzenesulfonyl-4-acetylamino-3-nitrobenzamide.

WORKUP

后处理

  1. stirringthe mixture was stirred at 100° C. for 72 hours
  2. customThe reaction mixture was separated with the addition of chloroform and water
  3. concentrationThe organic layer was then concentrated
  4. customthe resulting residue was purified through silica-gel column chromatography (eluent
  5. additiona mixture of ethyl acetate and methanol at a ratio of 4:1)