反应详情

19.7 g of laurolactam in 100 ml of chloroform were cooled to 0° C. 20.8 g of phosphorus pentachloride were added portionwise over a period of 40 minutes while keeping the temperature below 5° C. There was then added 0.2 g of iodine, followed by 16.0 g (0.2 mol) of bromine over a period of 20 minutes. The mixture was heated under reflux for 4 hours, cooled, evaporated and poured on to ice. The product was taken up in chloroform, washed with sodium hydrogen sulfate solution, dried over anhydrous magnesium sulfate and evaporated. Crystallization from chloroform/ n-hexane yielded 12.65 g (46%) of 3-bromolaurolactam of melting point 155°-157° C.

1. customthe temperature below 5° C
2. temperatureThe mixture was heated
3. temperatureunder reflux for 4 hours
4. temperaturecooled
5. customevaporated
6. additionpoured on to ice
7. washwashed with sodium hydrogen sulfate solution
8. dry with materialdried over anhydrous magnesium sulfate
9. customevaporated
10. customCrystallization from chloroform/ n-hexane