HRID362673

反应详情

EQUATION

反应方程式

HRID 362673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureThe temperature of the mixture was raised
  2. customto return to a temperature of 40° C.
  3. filtrationthe catalyst was filtered off
  4. customThe solvents were then removed under vacuum until 21.4 g of crude product
  5. customwere obtained which
  6. customThe crystals obtained
  7. washwashed with petroleum ether
  8. dry with materialdried under vacuum over phosphorus pentoxide