Реакция #2389092

ord-c1ec2326fbc845d3804303d03c208e5d

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

220 mg of tetrafluorophthalic anhydride and 127 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 210 mg of the desired product as a colorless powder. Yield: 64%. m.p. 147-148° C.; [α]20D=−5.13° (C=0.658 AcOEt); MS(EI+) 329(M)+

Источник

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