反应详情

To a slurry of 99 g of naphthalene (0.75 mole) and 96 g of isonipecotic acid chloride hydrochloride (0.5 mole) in tetrachloroethane is added over a period of 10 minutes 200 g (1.5 moles) of aluminum chloride. The reaction mixture is allowed to stand at room temperature for 10 minutes, then decomposed by pouring it over ice water, made basic with a 50% NaOH solution, and extracted with diethyl ether. The ether layer is dried over magnesium sulfate, filtered, and treated with ethereal HCl. The resulting oil is dissolved in warmed methanol, treated with charcoal, filtered and diluted with butanone. The methanol is removed by distillation, adding more butanone as needed. The solution is cooled overnight, and the resulting solid filtered off and recrystallized from methanol-butanone to give the desired product. M.P. 251°-253° C.

1. extractionextracted with diethyl ether
2. dry with materialThe ether layer is dried over magnesium sulfate
3. filtrationfiltered
4. additiontreated with ethereal HCl
5. dissolutionThe resulting oil is dissolved in warmed methanol
6. additiontreated with charcoal
7. filtrationfiltered
8. additiondiluted with butanone
9. customThe methanol is removed by distillation
10. additionadding more butanone
11. temperatureThe solution is cooled overnight
12. filtrationthe resulting solid filtered off
13. customrecrystallized from methanol-butanone