HRID611786

反应详情

EQUATION

反应方程式

HRID 611786 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 5% by weight palladium-on-charcoal, 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 brought to and maintained at 162° C. for 10 hours. The mixture was then allowed to return to a temperature of 40° C. and the catalyst was then 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 filtered off, washed with petroleum ether and then dried under vacuum over phosphorus pentoxide. 11 g of 4-hydroxy-1-N-(β-hydroxyethyl)indole were obtained, the melting point of which was 109° C.

WORKUP

后处理

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