Реакция #320375

ord-9c1cde608ff74529a27e9527933d49c7

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаwashed twice with 10% sodium hydroxide (200 ml), water, and brine
  2. 2
    Сушкаdried (Na2SO4)
  3. 3
    КонцентрированиеThe product was concentrated to an oil
  4. 4
    workup.STIRRINGA portion was stirred with ether (100 ml)
  5. 5
    Другоеa crystalline product was formed
  6. 6
    ФильтрацияThe crystalline product was recovered by filtration
  7. 7
    Другоеpurified by recrystallization

Методика

To the compound p-bromoacetophenone (36.85 g, 185 mmol) in trichloromethane (300 ml) was added 1,3-propanedithiol (25 g, 230 mmol) and boron trifluoride etherate (3 ml). The resulting mixture was stirred at room temperature for 48 hours. The mixture was diluted with dichloromethane (500 ml), washed twice with 10% sodium hydroxide (200 ml), water, and brine, and then dried (Na2SO4). The product was concentrated to an oil. A portion was stirred with ether (100 ml) and a crystalline product was formed. The crystalline product was recovered by filtration and purified by recrystallization to yield 4-bromo-1-(1,3-dithian-2-yl)ethylbenzene.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05591745uspto-grants-1997_01