Реакция #459737

Уравнение реакции

sulfuric acid

product

7-(4-methylpiperazin-1-yl)-5ξ-hydroxy-6,7,8,9-tetrahydro [5H] benzocycloheptene

→

7-(4-methylpiperazin-1-yl)-6,7-dihydro [5H] benzocycloheptene

Выход 74.0%

Растворители

dioxane

Условия реакции

Обработка

1. 1
   Температураthe mixture was refluxed for 30 minutes
2. 2
   Концентрированиеwas concentrated
3. 3
   workup.ADDITION100 ml of ice-water were added
4. 4
   Экстракцияthe mixture was extracted with ethyl acetate
5. 5
   Экстракцияwas extracted with methylene chloride
6. 6
   ДругоеThe organic phase was dried
7. 7
   Другоеevaporated to dryness

Методика

18 ml of 18 N sulfuric acid were added to a refluxing solution of 9 g of the product of Step B in 180 ml of dioxane and the mixture was refluxed for 30 minutes and then was concentrated and cooled to 20° C. 100 ml of ice-water were added thereto and the mixture was extracted with ethyl acetate. The aqueous phase was made alkaline with concentrated ammonium hydroxide and was extracted with methylene chloride. The organic phase was dried and evaporated to dryness to obtain 6.2 g of 7-(4-methylpiperazin-1-yl)-6,7-dihydro [5H] benzocycloheptene.

Источник