反应详情

Into a 5 L, 3 neck round bottom flask fitted with nitrogen inlet, condenser, thermometer, mechanical stiring and nitrogen outlet is added 6-bromo-1-hexanol (500 g, 2.76 mol), triphenylphosphine (768 g, 2.9 mol) and acetonitrile (1800 ml) under nitrogen. The reaction mixture is heated to reflux for 72 hrs. The reaction mixture is cooled to room temperature and transferred into a 5 L beaker. The product is recrystallized from anhydrous ethyl ether (1.5 L) at 10° C. Vacuum filtration followed by washing with ethyl ether and drying in a vacuum oven at 50° C. for 2 hrs. gives 1140 g of the desired product as white crystals.

1. customInto a 5 L, 3 neck round bottom flask fitted with nitrogen inlet, condenser
2. temperatureThe reaction mixture is heated
3. temperatureto reflux for 72 hrs
4. customThe product is recrystallized from anhydrous ethyl ether (1.5 L) at 10° C
5. filtrationVacuum filtration
6. washby washing with ethyl ether
7. customdrying in a vacuum oven at 50° C. for 2 hrs