HRID1777329

反应详情

EQUATION

反应方程式

HRID 1777329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of concentrated sulfuric acid & nitric acid (68-72%) (1.7:6, 15 mL) is added drop wise to a cold solution of 1-(4-cyclohexylphenyl)ethanone (6 g, 0.03 mol) in concentrated sulfuric acid (15 mL) at 0-5° C. Reaction mixture is allowed to stir at this temperature for 30 minutes & is then poured into crushed ice. It is then extracted with ethyl acetate (3×40 mL). Combined organic layer is dried over sodium sulfate and concentrated under reduced pressure. The residue is purified by column chromatography (silica gel, 230-400 mesh, ethyl acetate:n-hexane 1:9) to yield 1-(4-cyclohexyl-3-nitrophenyl)ethanone.

WORKUP

后处理

  1. customReaction mixture
  2. additionis then poured
  3. custominto crushed ice
  4. extractionIt is then extracted with ethyl acetate (3×40 mL)
  5. dry with materialCombined organic layer is dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue is purified by column chromatography (silica gel, 230-400 mesh, ethyl acetate:n-hexane 1:9)