Реакция #1944153

ord-1d87b34ef9fc4393b306389f506910a4

Реагенты

Нет

Растворители

Условия реакции

Температура
4°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGThe reaction mixture was stirred at 23° C. for 15 hours
  2. 2
    Другоеprecipitates
  3. 3
    Другоеformed
  4. 4
    ДругоеThe precipitates (triethylamine.HBr)
  5. 5
    Фильтрацияwere filtered out
  6. 6
    Концентрированиеthe filtrate was concentrated to dryness
  7. 7
    ДругоеThen the crude reaction mixture
  8. 8
    Другоеwas purified by column chromatography (SiO2, hexane/CH2Cl2 =5/1)

Методика

A mixture of 5-acenaphthylamine (1.0 g, 6 mmol) and triethylamine (0.76 g, 7.5 mmol) in toluene (50 mL) was stirred at 4° C., and 4-tert-butylbenzyl-bromide (1.36 g, 6 mmol) was added in slowly. The reaction mixture was stirred at 23° C. for 15 hours and precipitates formed. The precipitates (triethylamine.HBr) were filtered out; the filtrate was concentrated to dryness. Then the crude reaction mixture was purified by column chromatography (SiO2, hexane/CH2Cl2 =5/1). N-(5-acenaphthyl)-4-tert-butylbenzylamine (1.67 g, an oil) was obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06143791uspto-grants-2000_11