HRID2070580

反应详情

EQUATION

反应方程式

HRID 2070580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of potassium tert-butoxide (24.4 g) in toluene (100 mL) was added a solution of cyclohexanone (10.67 g) and 1,5-dibromopentane (25 g) in toluene (50 mL) while stirring. The mixture was stirred at 100° C. for 4 hours. After cooling down to room temperature, the resulting solid was filtered and washed with toluene. The filtrate was concentrated and the residue was purified by column chromatography on silica gel (ethyl acetate:hexane (volume ratio)=1:15) to give spiro[5.5]undecan-1-one (11.85 g).

WORKUP

后处理

  1. stirringThe mixture was stirred at 100° C. for 4 hours
  2. filtrationthe resulting solid was filtered
  3. washwashed with toluene
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by column chromatography on silica gel (ethyl acetate:hexane (volume ratio)=1:15)