Реакция #60087

Уравнение реакции

1-(2,4-dichlorophenyl)-2-chloroethan-1-one

imidazole

→

1-(2,4-dichlorophenyl)-2-imidazolylethan-1-one

Выход 90.0%

Растворители

CH3CN

dichloromethane

water

Условия реакции

Обработка

1. 1
   ФильтрацияAfter filtering off a solid impurity
2. 2
   Другоеthe aqueous layer was removed
3. 3
   ПромывкаThe organic layer was washed sequentially with water (300 ml), sat. aq. NaHCO3 (300 ml), water (300 ml), brine (200 ml)
4. 4
   Сушкаdried with Na2SO4
5. 5
   Фильтрацияfiltered
6. 6
   Концентрированиеconcentrated under reduced pressure
7. 7
   ДругоеThe reddish black oil was dried overnight in vacuo

Методика

A stirred solution of 1-(2,4-dichlorophenyl)-2-chloroethan-1-one (0.95 M) and imidazole (2.68 M) in CH3CN (500 ml) were heated for 14-16 hours at 75° C. The product was stripped of solvent under reduced pressure. The residue was diluted with dichloromethane (1 L) and water (400 ml), and the mixture was stirred for 30 min. After filtering off a solid impurity, the aqueous layer was removed and discarded. The organic layer was washed sequentially with water (300 ml), sat. aq. NaHCO3 (300 ml), water (300 ml), brine (200 ml), dried with Na2SO4, filtered, and concentrated under reduced pressure. The reddish black oil was dried overnight in vacuo giving 1-(2,4-dichlorophenyl)-2-imidazolylethan-1-one in 90% yield.

Источник