HRID46511

反应详情

EQUATION

反应方程式

HRID 46511 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The solution of 50 g of 2-cyanomethyl-6-methoxy-1-tetralone in 1000 ml of ethanol is hydrogenated in the presence of 15 g of Raney nickel at atmospheric pressure and room temperature until 2 mole equivalents of hydrogen are consumed. The mixture is filtered, the filtrate evaporated and the crude product dissolved in 500 ml of N hydrochloric acid. The solution is washed with diethyl ether, treated with charcoal, filtered and the filtrate is basified with 3 N aqueous sodium hydroxide. It is extracted with methylene chloride, the extract dried, evaporated, the residue crystallized from petroleum ether and recrystallized from hexane, to yield the 7-methoxy-3,3a,4,5-tetrahydro-2H-benz[g]indole melting at 102°-104°.

WORKUP

后处理

  1. customare consumed
  2. filtrationThe mixture is filtered
  3. customthe filtrate evaporated
  4. dissolutionthe crude product dissolved in 500 ml of N hydrochloric acid
  5. washThe solution is washed with diethyl ether
  6. additiontreated with charcoal
  7. filtrationfiltered
  8. extractionIt is extracted with methylene chloride
  9. customthe extract dried
  10. customevaporated
  11. customthe residue crystallized from petroleum ether
  12. customrecrystallized from hexane