HRID417876

反应详情

EQUATION

反应方程式

HRID 417876 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 (2.0 mL) and piperazine (2.0 g) in EtOH (6 mL) was heated to reflux for 30 min. The mixture was concentrated, diluted with NaOH 2 M (8 mL) and extracted with Et2O (50 mL). Evaporation of the organic layer gave a 2:1 mixture of mono and bis-alkylated piperazine (450 mg) which was discarded. The aqueous layer was further extracted with DCM (100 mL) to give of 1-(but-3-ynyl)piperazine (640 mg).

WORKUP

后处理

  1. temperatureto reflux for 30 min
  2. concentrationThe mixture was concentrated
  3. additiondiluted with NaOH 2 M (8 mL)
  4. extractionextracted with Et2O (50 mL)
  5. customEvaporation of the organic layer
  6. customgave
  7. extractionThe aqueous layer was further extracted with DCM (100 mL)