Реакция #44423

ord-a5c35d0dd7fe4a1aa842846ec4e1bb61

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураunder reflux for 5 h
  2. 2
    Фильтрацияthe mixture is filtered
  3. 3
    Концентрированиеthe filtrate is concentrated in vacuo
  4. 4
    workup.ADDITIONEthanol is added to the residue
  5. 5
    workup.STIRRINGthe mixture is stirred
  6. 6
    ФильтрацияThe solid is filtered off with suction
  7. 7
    Другоеdried

Методика

Metallic sodium (2.6 g, 113 mmol) is added to ethanol (60 ml). The mixture is stirred until the sodium has completely finished reacting. Diethyl malonate (116 ml, 105 mmol) and n-propylurea (10 g, 98 mmol) are then added and the mixture is stirred under reflux for 5 h. After conc. HCl (5 ml) and hot water (45 ml) have been added, the mixture is filtered and the filtrate is concentrated in vacuo. Ethanol is added to the residue and the mixture is stirred. The solid is filtered off with suction and dried.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07737144B2uspto-grants-2010_06