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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (2.0 g, 12.0 mmol), 1-(4-ethylphenyl)piperazine (2.36 g, 12.0 mmol), anhydrous Na2CO3 (0.658 g, 6.2 mmol) and NaI (0.18 g, 1.2 mmol) in dry DMF (10 ml) was stirred at 80° C. for 12 hrs. The reaction mixture was cooled, poured on water (30 ml) and the separated residue was extracted with CHCl3 (2×30 ml). The extracts were dried over Na2So4 and concentrated under reduced pressure to give 1-[4-(4-ethylphenyl)piperazin-1-yl]-3-[2-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as eluent, yield 2.43 g (62.0%). IR (Neat): 2940, 2800, 1660, 1440, 1000, 900,800. 1H NMR (CDCl3): 1.20(t, 3H, J=6.0 Hz, CH2CH3, 1.60-280(m, 14H, 3',4',2,1 & 2×N--CH2, CH2CH3), 3.00-3.60(m, 8H, 5', 3 & 2×N--CH2). MS: m/z 315 (M+).
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- additionpoured on water (30 ml)
- extractionthe separated residue was extracted with CHCl3 (2×30 ml)
- customThe extracts were dried over Na2So4
- concentrationconcentrated under reduced pressure