HRID2184803

反应详情

EQUATION

反应方程式

HRID 2184803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.7 g of Pd/C (10%) is added to a solution of 3.4 g of the product obtained in Step C and 4.4 g of ammonium formate in 150 ml of anhydrous methanol under a stream of argon. After refluxing for 45 minutes, the reaction mixture is cooled, 4.4 g of ammonium formate 5 and 0.2 g of Pd/C (10%) are added, and the reaction mixture is then heated at reflux for 30 minutes. After returning to ambient temperature, filtration over Celite and concentration under reduced pressure, the residue is taken up in water and then extracted with dichloromethane. The expected product is isolated by extraction, drying, filtration and concentration under reduced pressure.

WORKUP

后处理

  1. temperatureAfter refluxing for 45 minutes
  2. temperaturethe reaction mixture is cooled
  3. temperaturethe reaction mixture is then heated
  4. temperatureat reflux for 30 minutes
  5. customAfter returning to ambient temperature
  6. filtrationfiltration
  7. concentrationover Celite and concentration under reduced pressure
  8. extractionextracted with dichloromethane