HRID1984104

反应详情

EQUATION

反应方程式

HRID 1984104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1-(but-3-ynyl)piperazine (445 mg) in THF (4 mL) was treated with 4-nitrophenyl carbonochloridate (649 mg) at rt for 5 min. A precipitate formed immediately, and the suspension was treated with Et3N (0.45 mL) to ensure complete reaction. The suspension was diluted wiht H2O (2 mL), MeOH (2 mL) and 40% aq. MeNH2 (4.0 mL) and stirred at rt for 3 days. Extraction with DCM (50 mL), washing (NaOH 2M), drying (Na2SO4) and concentration gave 4-(but-3-ynyl)-N-methylpiperazine-1-carboxamide (370 mg).

WORKUP

后处理

  1. customA precipitate formed immediately
  2. customreaction
  3. extractionExtraction with DCM (50 mL)
  4. washwashing (NaOH 2M)
  5. customdrying
  6. concentration(Na2SO4) and concentration