Реакция #2069926

ord-8826973177f346569a29a8230f5bbb3c

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONThe ethanolic solution is poured into dist
  2. 2
    Фильтрацияwater, and the brownish precipitate is filtered off with suction
  3. 3
    workup.DISSOLUTIONdissolved in dichloromethane
  4. 4
    Сушкаdried with sodium sulphate
  5. 5
    КонцентрированиеThe solution is concentrated
  6. 6
    Другоеchromatographed through a short silica gel column with 50% dichloromethane in hexane
  7. 7
    КонцентрированиеThe product fractions are concentrated to dryness
  8. 8
    Другоеthe product is dried under reduced pressure

Методика

N-Acetyl-N,N-di(4-isopropylphenyl)amine (5.4 g, 18.4 mmol) are heated to reflux in 100 ml of 20% aqueous ethanol. The reaction is monitored by thin-layer chromatography. After 30 h, no reactant is any longer detectable in the TLC. The ethanolic solution is poured into dist. water, and the brownish precipitate is filtered off with suction, dissolved in dichloromethane and dried with sodium sulphate. The solution is concentrated and chromatographed through a short silica gel column with 50% dichloromethane in hexane. The product fractions are concentrated to dryness and the product is dried under reduced pressure.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07540978B2uspto-grants-2009_06