HRID1909357

反应详情

EQUATION

反应方程式

HRID 1909357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Pd/C 10% (169 mg, 159 μmol,) was added to a solution of 4-(benzo[1,3]dioxol-4-yl)-1,2,3,6-tetrahydropyridine hydrochloride (760 mg, 3.17 mmol) and ammonium formate (1.00 g, 15.9 mmol) in methanol (28.8 ml) under argon. After refluxing for 60 min the reaction mixture was cooled to room temperature, filtrated and concentrated under reduced pressure. Saturated sodium bicarbonate solution was added to the residue and the mixture was extracted with dichloromethane (3×25 mL). The organic layers were dried over MgSO4 and concentrated in vacuo to yield the title compound as a white solid (0.654 grs, 100%). MS (ISP) m/z=206.0[(M+H)+].

WORKUP

后处理

  1. temperatureAfter refluxing for 60 min the reaction mixture
  2. filtrationfiltrated
  3. concentrationconcentrated under reduced pressure
  4. additionSaturated sodium bicarbonate solution was added to the residue
  5. extractionthe mixture was extracted with dichloromethane (3×25 mL)
  6. dry with materialThe organic layers were dried over MgSO4
  7. concentrationconcentrated in vacuo