HRID1777332

反应详情

EQUATION

反应方程式

HRID 1777332 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

An aqueous alkaline solution of potassium permanganate (2.94 g, 0.0186 mol; in 22 mL 12% aqueous sodium hydroxide) is added to solution of 1-(3-chloro-4-cyclohexylphenyl)ethanone (2.2 g, 0.0093 mol) in dioxane (11 mL). The reaction mixture is stirred at 80° C. temperature for 2 hrs. It is then filtered and the filtrate is washed with diethyl ether (2×10 mL). The pH of the aqueous layer is adjusted to 1-2 by using 6N hydrochloric acid. It is extracted in ethyl acetate (3×15 mL). Combined organic layer is dried over sodium sulfate and concentrated to get the crude, which is purified using column chromatography (230-400 mesh; ethyl acetate:n-hexane, 1:3) to yield 3-chloro-4-cyclohexyl benzoic acid.

WORKUP

后处理

  1. filtrationIt is then filtered
  2. washthe filtrate is washed with diethyl ether (2×10 mL)
  3. extractionIt is extracted in ethyl acetate (3×15 mL)
  4. dry with materialCombined organic layer is dried over sodium sulfate
  5. concentrationconcentrated
  6. customto get the crude, which
  7. customis purified