Реакция #6702

ord-c0b1f5fc553446359bccb5846409ec6d

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThis solution was washed twice with aqueous bicarbonate
  2. 2
    Сушкаdried over magnesium sulfate
  3. 3
    Концентрированиеconcentrated under reduced pressure
  4. 4
    ДругоеA colorless oil was recovered

Методика

4-Bromobenzaldehyde (3 g, 0.0162 mol) in benzene (60 mL) was treated with p-toluenesulfonic acid monohydrate (0.15 g, 0.79 mmol) and ethylene glycol (5 mL, 0.0896 mol). The reaction was refluxed under nitrogen with azeotropic removal of water. After 3 hours, the reaction was cooled to room temperature and diluted with an equal volume of ethyl acetate. This solution was washed twice with aqueous bicarbonate, dried over magnesium sulfate and concentrated under reduced pressure. A colorless oil was recovered. Yield=2.83 g (92%). TLC (5% ethyl acetate in hexanes) showed clean product, Rf=0.17.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07083986B2uspto-grants-2006_08