HRID1059135

反应详情

EQUATION

反应方程式

HRID 1059135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 1-(4-bromophenyl)-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol (3.60 g), 4-fluorophenylboronic acid (1.50 g) and 2M aqueous sodium carbonate solution (26.8 ml) in dimethoxyethane (50 ml) was added tetrakis(triphenylphosphine)palladium(0) (387 mg). Under an argon atmosphere, the mixture was heated under reflux for 12 h. The reaction mixture was extracted with ethyl acetate-THF (8:3), washed with water and saturated brine, and dried. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chomatography (eluent, hexane:ethyl acetate=6:1→4:1) to give the title compound (3.16 g) as colorless needle crystals.

WORKUP

后处理

  1. temperatureUnder an argon atmosphere, the mixture was heated
  2. temperatureunder reflux for 12 h
  3. extractionThe reaction mixture was extracted with ethyl acetate-THF (8:3)
  4. washwashed with water and saturated brine
  5. customdried
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by silica gel column chomatography (eluent, hexane:ethyl acetate=6:1→4:1)