HRID2220606

反应详情

EQUATION

反应方程式

HRID 2220606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A mixture of 4-bromo-2-isopropylphenyl trifluoromethanesulfonate (0.705 g), palladium acetate (0.0228 g), 1,3-bis-(diphenylphosphino)propane (0.0419 g) and triethylamine (0.628 mL) in methanol (6 mL)/dimethylsulfoxide (9 mL) was stirred at 55° C. overnight under an atmosphere of carbon monoxide. Water and ethyl acetate were added to the reaction mixture. The organic layer was separated, washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: diethyl ether/n-hexane=1/10) to afford methyl 4-bromo-2-isopropylbenzoate (0.355 g).

WORKUP

后处理

  1. customThe organic layer was separated
  2. washwashed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (eluent: diethyl ether/n-hexane=1/10)