HRID2070436

反应详情

EQUATION

反应方程式

HRID 2070436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution (35 mL) of ethyl 5-(2,6-difluorophenyl)-1H-pyrrole-3-carboxylate (3.35 g) in tetrahydrofuran was cooled to −50° C., and a 1.5 mol/L solution (30 mL) of diisobutylaluminum hydride in toluene was added dropwise by small portions. The mixture was stirred at the same temperature for 1 hr, water was added to the reaction mixture, and the mixture was stirred at room temperature for 1 hr. The reaction mixture was diluted with ethyl acetate, celite and anhydrous magnesium sulfate were added and the mixture was further stirred for 15 min. The suspension was filtrated, and the obtained filtrate was concentrated under reduced pressure to give the title compound as pale-red crystals (yield 2.70 g, 97%).

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 1 hr
  2. additionwere added
  3. stirringthe mixture was further stirred for 15 min
  4. filtrationThe suspension was filtrated
  5. concentrationthe obtained filtrate was concentrated under reduced pressure