HRID483187

反应详情

EQUATION

反应方程式

HRID 483187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.8 Grams of 2-(4-chlorobenzoylamino)-3-(2-quinolon-4-yl)propionic acid was dissolved in 80 ml of N,N-dimethylformamide. To this solution was added 0.6 g of triethylamine. Then, under ice-cooled condition with stirring, 0.8 g of isobutyl chloroformate was added to the above-mentioned mixture. At the same temperature condition, 10 ml of N,N-dimethylformamide solution containing 0.4 g of ammonia was added dropwise to the reaction mixture, and stirred for 3 hours. After the removal of N,N-dimethylformamide by distillation, water was added to the residue and the crystals precipitated were collected by filtration, and were washed with an aqueous solution of sodium hydroxide. Recrystallized from dimethylformamide-water to obtain 0.7 g of 2-(4-chlorobenzoylamino)-3-(2-quinolon-4-yl)propionamide in the form of light yellowish powdery product.

WORKUP

后处理

  1. temperatureThen, under ice-cooled condition
  2. additionwas added dropwise to the reaction mixture
  3. stirringstirred for 3 hours
  4. customAfter the removal of N,N-dimethylformamide
  5. distillationby distillation, water
  6. additionwas added to the residue
  7. customthe crystals precipitated
  8. filtrationwere collected by filtration
  9. washwere washed with an aqueous solution of sodium hydroxide
  10. customRecrystallized from dimethylformamide-water