反应 #1755

ord-d5a8195f23794884af3a23a8c8f6148d

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the mixture is extracted with methylene chloride
  2. 2
    其他The organic phase is dried
  3. 3
    其他evaporated down in vacuo
  4. 4
    其他the residue remaining is purified by column chromatography (aluminium oxide basic, activity stage III, ICN; petroleum ether/ethyl acetate=15:1)

实验过程

A solution of 1 g (3.75 mmol) of trans-O-acetyl-4-(4-chloromethylphenyl)-cyclohexanol in 10 ml of dimethylformamide is mixed with 0.52 g (3.75 mmol) of potassium carbonate and 0.27 g (3.75 mmol) of diethylamine. This mixture is heated to 50° C. for 6 hours with stirring, then water is added and the mixture is extracted with methylene chloride. The organic phase is dried, evaporated down in vacuo and the residue remaining is purified by column chromatography (aluminium oxide basic, activity stage III, ICN; petroleum ether/ethyl acetate=15:1). Colourless oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726205uspto-grants-1998_03