反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 162 °C
PROCEDURE
实验过程
15 g of palladium on carbon at 5% by weight and containing 50% of water were added to a solution of 25 g of 4-oxo-4,5,6,7-tetrahydro-1-N-(β-hydroxyethyl)indole, obtained in the preceding stage, in 300 cm3 of diglyme. The temperature of the mixture was raised and maintained at 162° C. for 10 hours. The mixture was then allowed to return to a temperature of 40° C. and then the catalyst was filtered off. The solvents were then removed under vacuum until 21.4 g of crude product were obtained which were taken up in a mixture of 30 cm3 of dichloromethane and 200 cm3 of petroleum ether. The crystals obtained were drained, washed with petroleum ether and then dried under vacuum over phosphorus pentoxide. 11 g of 4-hydroxy-1-N-(β-hydroxyethyl)indole were obtained whose elemental analysis, calculated for C10H11NO2, was:
WORKUP
后处理
- temperatureThe temperature of the mixture was raised
- customto return to a temperature of 40° C.
- filtrationthe catalyst was filtered off
- customThe solvents were then removed under vacuum until 21.4 g of crude product
- customwere obtained which
- customThe crystals obtained
- washwashed with petroleum ether
- dry with materialdried under vacuum over phosphorus pentoxide