HRID1077421

反应详情

EQUATION

反应方程式

HRID 1077421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Propanal (1.51 g) dissolved in 5 ml of methanol was added dropwise to 6.15 g of 2-aminomethyl-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane dissolved in 60 ml of methanol. The mixture was stirred at room temperature for 30 minutes. Then, under ice cooling, 1.03 g of sodium borohydride was added to the mixture. The resulting mixture was stirred at the same temperature for 20 minutes and then stirred at room temperature for 1 hour. After methanol was removed, water was added to the residue, and the residue was extracted with ethyl acetate. The organic layer was collected by filtration, washed with water and dried, and the solvent was removed. The residue was purified by silica gel column chromatography (solvent; chloroform: methanol (15:1)) to obtain 5.22 g of 2-propylaminomethyl-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane.

WORKUP

后处理

  1. stirringThe resulting mixture was stirred at the same temperature for 20 minutes
  2. stirringstirred at room temperature for 1 hour
  3. customAfter methanol was removed
  4. additionwater was added to the residue
  5. extractionthe residue was extracted with ethyl acetate
  6. filtrationThe organic layer was collected by filtration
  7. washwashed with water
  8. customdried
  9. customthe solvent was removed
  10. customThe residue was purified by silica gel column chromatography (solvent; chloroform: methanol (15:1))