HRID1170089

反应详情

EQUATION

反应方程式

HRID 1170089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[(5-Methyl-furan-2-ylmethyl)-amino]-quinoline-5-carbaldehyde (100 mg, 0.376 mmol) was dissolved in 5 mL ethylendichloride. 3-Aminopyridine (50 mg, 0.532 mmol) and acetic acid (90 mg, 1.50 mmol) were added. The reaction mixture was stirred at room temperature for 1 h. Sodium triacetoxy borohydride (172 mg, 0.811 mmol) was added and stirring was continued overnight. The reaction mixture was quenched by addition of 50 mL water. The mixture was extracted three times with dichloromethane (50 mL each). The organic phases ware pooled, dried with sodium sulfate, filtered and evaporated. The crude product was recrystallized from dichloromethane. The title compound was obtained as a white solid (50 mg, 39%), MS: m/e=345.0 (M+H+).

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued overnight
  3. customThe reaction mixture was quenched by addition of 50 mL water
  4. extractionThe mixture was extracted three times with dichloromethane (50 mL each)
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customThe crude product was recrystallized from dichloromethane