HRID1855655

反应详情

EQUATION

反应方程式

HRID 1855655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

In a Parr bomb under a hydrogen pressure of 6 bar, 100 mg of rhodium on alumina and 0.2 ml of acetic acid are added to a solution of 100 mg (0.5 mmol) of 4-butyryl-4-phenylpiperidine hydrochloride in 10 ml of dioxane. The reaction medium is heated at 80° C. for 12 hours. The reaction is stopped and then filtered through Celite and washed with dichloromethane. The solvents are evaporated off and the residue is taken up in water, basified with 1N sodium hydroxide solution and extracted with ethyl acetate. The organic phases are dried over sodium sulfate. The solvents are evaporated off and the residue is chromatographed on silica gel (eluent: 9/1 dichloromethane/methanol). 51.2 mg of 1-(4-cyclohexylpiperidin-4-yl)-butan-1-one in the form of a white powder are obtained in a yield of 61%.

WORKUP

后处理

  1. filtrationfiltered through Celite
  2. washwashed with dichloromethane
  3. customThe solvents are evaporated off
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phases are dried over sodium sulfate
  6. customThe solvents are evaporated off
  7. customthe residue is chromatographed on silica gel (eluent: 9/1 dichloromethane/methanol)