HRID1276877

反应详情

EQUATION

反应方程式

HRID 1276877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N,N'-carbonyldiimidazole (28.9 g) was added to a solution of 20.0 g of 3-acetylamino-4-nitrobenzoic acid in 300 ml of N,N-dimethylformamide, and the mixture was stirred at room temperature for 1 hour. Further, 28.00 g of benzenesulfonamide and 27.16 g of diazabicycloundecene were added thereto, and the mixture was stirred at 100° C. for 4 days. The solvent was distilled off under reduced pressure. Chloroform and a 10% sodium hydroxide aqueous solution were added to the residue, and the mixture was vigorously stirred. The aqueous layer was neutralized with 10% hydrochloric acid, and the mixture was vigorously stirred with the addition of chloroform. The crystals precipitated were separated through filtration, and were dried to 14.4 g of N-benzenesulfonyl-3-amino-4-nitrobenzamide.

WORKUP

后处理

  1. stirringthe mixture was stirred at 100° C. for 4 days
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionChloroform and a 10% sodium hydroxide aqueous solution were added to the residue
  4. stirringthe mixture was vigorously stirred
  5. stirringthe mixture was vigorously stirred with the addition of chloroform
  6. customThe crystals precipitated
  7. customwere separated through filtration
  8. dry with materialwere dried to 14.4 g of N-benzenesulfonyl-3-amino-4-nitrobenzamide