反应 #54465

反应方程式

ammonium chloride

magnesium

methallyl chloride

2-acetyl-3,3-dimethyl-5-norbornene

→

oil

收率 106.5%

ALPHA-METHALLYL-ALPHA,3,3-TRIMETHYL-5-NORBORNENE-2-METHANOL

收率 106.5%

溶剂

diethyl ether

反应条件

后处理

1. 1
   其他Into a 1 liter reaction flask
2. 2
   其他equipped with a reflux condenser
3. 3
   其他thermometer, stirrer, dropping
4. 4
   其他funnel and nitrogen inlet tube are placed
5. 5
   workup.STIRRINGThe mixture is stirred
6. 6
   温度at reflux for 1/2 hour
7. 7
   洗涤The organic layer is washed with water
8. 8
   干燥dried over magnesium sulfate
9. 9
   过滤The mixture is then filtered
10. 10
    其他the solvent evaporated

实验过程

Into a 1 liter reaction flask equipped with a reflux condenser, thermometer, stirrer, dropping funnel and nitrogen inlet tube are placed 12 g (0.5 moles) of magnesium turnings and 250 cc anhydrous diethyl ether. Over a 2 hour period, 45.3 g (0.5 moles) of methallyl chloride is added. The Grignard solution is stirred for 1/2 hour and 28 g of 2-acetyl-3,3-dimethyl-5-norbornene is added over a 20 minute period. The mixture is stirred at reflux for 1/2 hour and then is hydrolyzed by the addition of saturated ammonium chloride solution. The organic layer is washed with water and dried over magnesium sulfate. The mixture is then filtered and the solvent evaporated to yield 40 g of an oil, which is then fractionated on a micro Vigreux column after adding thereto 5 g Primol® and a trace quantity of Ionox®.

来源