HRID24507

反应详情

EQUATION

反应方程式

HRID 24507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-[2-(2-Oxo-1,2-dihydroindol-3-ylidenemethyl)-4,5,6,7-tetrahydro-1H-indol-3-yl]-propionic acid (10 g) was dissolved in 100 mL of dimethylformamide. Carbonyldiimidazole (6.3 g) was added and the mixture stirred at ambient temperature for 1 hour. Dimethylamine (2.7 g) and 30 mL of dimethylformamide were added and the stirring continued overnight at room temperature. Fifty mL of water was added to the mixture and stirring was continued for 10 minutes. The precipitate was collected by vacuum filtration, washed with 20 mL of water and then 20 mL of ethanol. The solid was slurry-washed in 30 mL of refluxing ethanol for 5 minutes and cooled to room temperature. The solid was collected by vacuum filtration, washed with 20 mL of ethanol and vacuum dried to give 8.9 g (83% yield) of N,N-dimethyl-3-[2-(2-oxo-1,2-dihydroindol-3-ylidenemethyl)-4,5,6,7-tetrahydro-1H-indol-3-yl]-propionamide.

WORKUP

后处理

  1. customthe stirring continued overnight
  2. customat room temperature
  3. stirringstirring
  4. waitwas continued for 10 minutes
  5. filtrationThe precipitate was collected by vacuum filtration
  6. washwashed with 20 mL of water
  7. washThe solid was slurry-washed in 30 mL of refluxing ethanol for 5 minutes
  8. temperaturecooled to room temperature
  9. filtrationThe solid was collected by vacuum filtration
  10. washwashed with 20 mL of ethanol and vacuum
  11. customdried