반응 #54465

반응 방정식

ammonium chloride

magnesium

methallyl chloride

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

→

oil

수율 106.5%

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

수율 106.5%

용매

diethyl ether

반응 조건

후처리

1. 1
   기타Into a 1 liter reaction flask
2. 2
   기타equipped with a reflux condenser
3. 3
   기타thermometer, stirrer, dropping
4. 4
   기타funnel and nitrogen inlet tube are placed
5. 5
   workup.STIRRINGThe mixture is stirred
6. 6
   온도at reflux for 1/2 hour
7. 7
   세척The organic layer is washed with water
8. 8
   건조dried over magnesium sulfate
9. 9
   여과The mixture is then filtered
10. 10
    기타the solvent evaporated

실험 절차

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®.

출처