反应详情

In a one litre reaction vessel, equipped with a stirrer, a cooler and a dropping funnel, 26.4 g magnesium, 100 g tetrahydrofurane and 1 g allyl chloride were heated to about 40° C. to start the reaction. A mixture of 76.5 g allyl chloride, 250 g tetrahydrofurane and 150 g tricyclo [5,2,1,02,6 ] decan-8-one was added in four hours, keeping the temperature at 35°-40° C. The reaction mixture was stirred for an additional 30 minutes and subsequently poured into a mixture of 600 g of ice and 80 g of acetic acid. The layers were separated and the water layer extracted twice with toluene. The combined organic layers were washed with 5% soda solution until alkaline and subsequently with water until neutral. The organic solvent was removed by distillation under reduced pressure. The residue was distilled on a Vigreux head at 2 mm.Hg. The fraction boiling between 93° and 95° C. was collected. Yield: 80%, nD20 : 1.5154.

1. customIn a one litre reaction vessel
2. customequipped with a stirrer
3. customthe reaction
4. additionwas added in four hours
5. customat 35°-40° C
6. customThe layers were separated
7. extractionthe water layer extracted twice with toluene
8. washThe combined organic layers were washed with 5% soda solution until alkaline and subsequently with water until neutral
9. customThe organic solvent was removed by distillation under reduced pressure
10. distillationThe residue was distilled on a Vigreux head at 2 mm.Hg
11. customboiling between 93° and 95° C.
12. customwas collected