Реакция #2389094

ord-a1fbca80a68742168f9738b613b55c2c

Реагенты

Нет

Растворители

Условия реакции

Температура
180°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooled
  2. 2
    Другоеpurified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v)
  3. 3
    Другоеrecrystallized 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)+

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06429212B1uspto-grants-2002_08