HRID1600200

反应详情

EQUATION

反应方程式

HRID 1600200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, in a round-bottom flask equipped with a refluxcondenser were placed 400 mg (1.7 mmol) of the above nitrile and 10 ml of formic acid. To the system were added ca. 500 mg of Raney nickel and the mixture was heated at reflux for 6 hours and stirred at room temperature overnight. The mixture was filtered through a pad of a diatomaceous earth,and the pad was rinsed with water and CHCl3. The layers were separatedand the aqueous phase was extracted with three portions of CHCl3. The combined organic fractions were dried and concentrated to obtain 270 mg ofthe title compound.

WORKUP

后处理

  1. customUnder a nitrogen atmosphere, in a round-bottom flask equipped with a refluxcondenser
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 6 hours
  4. filtrationThe mixture was filtered through a pad of a diatomaceous earth,and the pad
  5. washwas rinsed with water and CHCl3
  6. extractionwas extracted with three portions of CHCl3
  7. customThe combined organic fractions were dried
  8. concentrationconcentrated