Реакция #76408

ord-d0dced9652c940f7b799947c5aa9486a

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONis added dropwise
  2. 2
    Другоеthe temperature between 0 and 2° C.
  3. 3
    workup.WAITthe yellow mixture is further stirred 2 h at the same temperature
  4. 4
    ДругоеThe phases are separated
  5. 5
    Промывкаthe organic layer is washed with brine
  6. 6
    Сушкаdried over magnesium sulfate
  7. 7
    Другоеevaporated

Методика

Acetonitrile (25 ml) is added to a solution of potassium carbonate (3.45 g; 0.025 mol) in 15 ml of water and the mixture is cooled to 0° C. 4-Methoxycinnamaldehyde (8.1 g; 0.05 mol) dissolved in acetonitrile (25 ml) is added dropwise under efficient stirring over 30 min, keeping the temperature between 0 and 2° C., and the yellow mixture is further stirred 2 h at the same temperature. The phases are separated, the organic layer is washed with brine, dried over magnesium sulfate, and evaporated. The crude benzoic acid 1-cyano-3-(4-methoxyphenyl)-allyl ester (15 g), obtained as a pale yellow oil, is used for the next step without further purification.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06703182B1uspto-grants-2004_03