HRID1984104
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customA precipitate formed immediately
- customreaction
- extractionExtraction with DCM (50 mL)
- washwashing (NaOH 2M)
- customdrying
- concentration(Na2SO4) and concentration