HRID1984094

反应详情

EQUATION

反应方程式

HRID 1984094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of but-3-ynyl 4-methylbenzenesulfonate (1.72 g), N-phenyl piperazine (1.17 mL) and diisoproylethylamine (1.45 mL) in 1,2-dichloroethane (5 mL) was heated to reflux overnight. The mixture was concentrated, diluted with sat. aq. NaHCO3 (5 mL) and extracted with DCM (2×50 mL). Drying (Na2SO4) and silica gel flash chromatography (3% Et3N in EtOAc) afforded 1-(but-3-ynyl)-4-phenylpiperazine (0.76 g)

WORKUP

后处理

  1. temperatureto reflux overnight
  2. concentrationThe mixture was concentrated
  3. additiondiluted with sat. aq. NaHCO3 (5 mL)
  4. extractionextracted with DCM (2×50 mL)
  5. dry with materialDrying (Na2SO4) and silica gel flash chromatography (3% Et3N in EtOAc)