反应 #2460305

反应方程式

2-(1-naphthy)ethanol

triethylamine

dichloromethane

methacryloyl chloride

→

2-(1-naphthyl)ethyl methacrylate

溶剂

diethyl ether

反应条件

后处理

1. 1
   温度heated
2. 2
   温度at refluxed for 4 h
3. 3
   温度The reaction mixture was cooled to ambient and
4. 4
   过滤The solution was filtered
5. 5
   洗涤the filtrate was washed twice with water, once with NaHCO3
6. 6
   干燥The solution was dried (Na2SO4)
7. 7
   浓缩concentrated
8. 8
   workup.DISTILLATIONThe product was purified by distillation at reduced pressure
9. 9
   其他collecting the fraction bp 120-125° C./0.08 mm
10. 10
    其他to provide a colorless oil, mass

实验过程

A solution of 2-(1-naphthy)ethanol (30.0 g, 174 mmol), triethylamine (24.2 g, 239 mmol), 4-(dimethylamino)pyridine (1.1 g, 9.1 mmol), and dichloromethane (500 mL) was treated dropwise under nitrogen with methacryloyl chloride (18.9 g, 181 mmol), and then heated at refluxed for 4 h. The reaction mixture was cooled to ambient and diluted with diethyl ether. The solution was filtered and the filtrate was washed twice with water, once with NaHCO3, and once with brine. The solution was dried (Na2SO4) and concentrated to deposit a yellow oil. The product was purified by distillation at reduced pressure, collecting the fraction bp 120-125° C./0.08 mm to provide a colorless oil, mass: 36.0 g (86% theory). 1H (CDCl3): δ 2.00 (s, 3H), 3.50 (t, 2H), 4.55 (t, 2H), 5.60 (s, 1H), 6.15 (s, 1H), 7.50 (m, 4H), 7.8 (d, 1H), 7.9 (d, 1H), 8.2 (d, 1H).

来源