HRID1293141

反应详情

EQUATION

反应方程式

HRID 1293141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 3-mercapto-1H-1,2,4-triazole (1.15 g) and N,N-dimethylformamide (15 ml) was added 60% sodium hydride (450 mg). After foaming was completed, N-chlorosuccinimide in small portions was added to the mixture on an ice bath, and stirred at this temperature for 15 minutes. 2-methylimidazo[1,2-a]pyridine (1.0 g) was then added, and the reaction mixture was heated and stirred at room temperature for 1 hour, and then for 3 hours on an oil bath at 70° C. The reaction solution was concentrated under reduced pressure. The residue was washed twice with diethyl ether, and methanol was added to the residue to remove undissolved materials. The filtrate was concentrated, and then crystals precipitated by the addition of water were collected by filtration, washed with water, followed by diethyl ether, and dried to yield the title compound (480 mg).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. stirringstirred at room temperature for 1 hour
  3. waitfor 3 hours on an oil bath at 70° C
  4. concentrationThe reaction solution was concentrated under reduced pressure
  5. washThe residue was washed twice with diethyl ether, and methanol
  6. additionwas added to the residue
  7. customto remove undissolved materials
  8. concentrationThe filtrate was concentrated
  9. customcrystals precipitated by the addition of water
  10. filtrationwere collected by filtration
  11. washwashed with water
  12. customdried