反应详情

46.7 g (0.358 mol) of 2-chloro-1-formylcyclopent-1-ene are dissolved in 400 ml of toluene. 138 g (0.716 mol) of N-benzylglycine ethyl ester are added. The mixture is refluxed for one hour, the water of reaction being separated off via a water separator. After cooling, any precipitate formed is filtered off with suction and the toluene solution is washed with water, dried and concentrated. The residue is taken up in 300 ml of ethanol, 600 ml of 2N hydrochloric acid are added and the mixture is extracted 3× with petroleum ether. The petroleum ether phase is washed with 2×175 ml of ethanol/2N hydrochloric acid 1:2 and then with 100 ml of saturated NaHCO3 solution, the organic phase is dried over MgSO4, stirred with active charcoal and filtered with suction, and the filtrate is evaporated in vacuo. Yield: 53.1 g of oil.

1. temperatureThe mixture is refluxed for one hour
2. custombeing separated off via a water separator
3. temperatureAfter cooling
4. customany precipitate formed
5. filtrationis filtered off with suction
6. washthe toluene solution is washed with water
7. customdried
8. concentrationconcentrated
9. addition600 ml of 2N hydrochloric acid are added
10. extractionthe mixture is extracted 3× with petroleum ether
11. washThe petroleum ether phase is washed with 2×175 ml of ethanol/2N hydrochloric acid 1:2
12. dry with materialwith 100 ml of saturated NaHCO3 solution, the organic phase is dried over MgSO4
13. filtrationfiltered with suction
14. customthe filtrate is evaporated in vacuo