Реакция #2389094
ord-a1fbca80a68742168f9738b613b55c2c
Уравнение реакции
Реагенты
Нет
Растворители
Условия реакции
Температура
180°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ТемператураAfter cooled
- 2Другоеpurified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v)
- 3Другоеrecrystallized from a mixed solvent of n-hexane-ethyl acetate
Методика
386 mg of 3-nitrophthalic anhydride and 242 mg of (R)-α-methylbenzylamine were charged in an egg-plant type flask of 50 ml, followed by stirring under heating at a temperature of 180° C. for 1.5 hours. After cooled, the reaction product was dissolved in chloroform, purified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v), recrystallized from a mixed solvent of n-hexane-ethyl acetate, to obtain 430 mg of the desired product as a light yellow powder. Yield: 73%. m.p. 115-117° C.; MS(EI+) 296(M)+