HRID651959

反应详情

EQUATION

反应方程式

HRID 651959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A benzene solution of 180 g (1.5 moles) of mesitylene, 90 g of aluminum chloride and 13 g of nickel dichloride was stirred at 70° C. to 80° C. Simultaneously, 125 ml of formic acid was added dropwise to 230 ml of chlorosulfonic acid to generate carbon monoxide and hydrogen chloride gas which were blown into the above benzene solution for 6 hours. Next, water and ethyl acetate were added to the solution which was separated into an organic and an aqueous layer. The organic layer was washed with an aqueous solution of sodium chloride, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=8/1) to give 34.5 g (0.233 mole) of 2,4,6-trimethylbenzaldehyde as a colorless oil.

WORKUP

后处理

  1. customwas separated into an organic and an aqueous layer
  2. washThe organic layer was washed with an aqueous solution of sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=8/1)