HRID623738

反应详情

EQUATION

反应方程式

HRID 623738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

KOt-Bu (265 mg, 2.36 mmol) and 18-crown-6 (catalytic amount) were added to ethyl 3-(4-chlorophenyl)-5-(trifluoromethyl)-1H-pyrrole-2-carboxylate [for synthesis see ACI-06] (500 mg, 1.57 mmol) in dry THF (5 mL). The reaction mixture was stirred for 30 min. and 1-(bromomethyl)-3-chlorobenzene (647 mg, 3.15 mmol) was added to the reaction mixture. The reaction mixture was stirred at reflux temperature overnight. The reaction mixture was acidified with aqueous 1M KHSO4 (4 mL), diluted with H2O (4 mL) and extracted with EtOAc (50 mL). The organic layer was washed with brine, dried (Na2SO4), and concentrated to give crude product as a colourless oil (732 mg).

WORKUP

后处理

  1. customfor synthesis
  2. stirringThe reaction mixture was stirred
  3. temperatureat reflux temperature overnight
  4. extractionextracted with EtOAc (50 mL)
  5. washThe organic layer was washed with brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated