Реакция #459730

Уравнение реакции

sodium borohydride

product

7-methylamino-5-oxo-6,7,8,9-tetrahydro [5H] benzocycloheptene

→

7-methylamino-5-hydroxy-6,7,8,9-tetrahydro [5H] benzocycloheptene

Выход 104.2%

Растворители

water

ethanol

Условия реакции

Обработка

1. 1
   Концентрированиеwas concentrated to 500 ml
2. 2
   workup.ADDITIONThe mixture was poured into 2 liters of aqueous sodium chloride solution
3. 3
   Экстракцияthe mixture was extracted with ethyl acetate
4. 4
   ПромывкаThe organic phase was washed with aqueous sodium chloride solution
5. 5
   Другоеdried
6. 6
   Другоеevaporated to dryness

Методика

A solution of 47.5g of sodium borohydride in 475 ml of water was slowly added to a solution of 47.5 g of the product of Step A in 2.4 liters of ethanol and the mixture was stirred for 2 1/2 hours and then was concentrated to 500 ml. The mixture was poured into 2 liters of aqueous sodium chloride solution and the mixture was extracted with ethyl acetate. The organic phase was washed with aqueous sodium chloride solution, dried and evaporated to dryness to obtain 50 g of raw 7-methylamino-5-hydroxy-6,7,8,9-tetrahydro [5H] benzocycloheptene which was used as is for the next step.

Источник