反应 #2487415

反应方程式

2-Hydroxyethyl methacrylate

succinic anhydride

Triethylamine

→

liquid

收率 77.8%

4-(2-(Methacryloyloxy)ethoxy)-4-oxobutanoic Acid

收率 77.8%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   温度the reaction mixture was refluxed for 1.5 hours
2. 2
   洗涤washed with 2 M HCl (150 mL)
3. 3
   其他The organic phase was separated from the aqueous phase
4. 4
   干燥dried (MgSO4 and Na2SO4)
5. 5
   其他evaporated to dryness

实验过程

2-Hydroxyethyl methacrylate (25 g, 0.195 mol) and succinic anhydride (19.5 g, 0.195 mol) were added to dichloromethane (200 mL) under nitrogen. Triethylamine (28.5 ml, 20.72 g, 1.05 equiv.) was then added dropwise over 20 minutes and the reaction mixture was refluxed for 1.5 hours. The reaction mixture was then diluted with dichloromethane (200 mL), washed with 2 M HCl (150 mL) and then finally with brine (100 mL). The organic phase was separated from the aqueous phase, dried (MgSO4 and Na2SO4) and evaporated to dryness, yielding a viscous, colourless liquid (34.9 g, 77.8% yield). 1H NMR δ 1.89 (s, 3H, CH3), 2.59-2.67 (m, 4H, 2×CH2CO), 4.31 (br. s, 4H, 2×CH2OCO), 5.55 (s, 1H, vinyl CH), 6.08 (s, 1H, vinyl CH). 13C NMR δ 17.96, 28.64, 28.73, 62.15, 62.29, 126.12, 135.79, 167.11, 171.90, 177.73.

来源