HRID380375

反应详情

EQUATION

反应方程式

HRID 380375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of intermediate (2) (0.067 mol) and KOH (0.67 mol) in 2-propanol (250 ml) was stirred and refluxed for 5 hours. The solvent was evaporated. Water (300 ml) was added and the organic solvent was removed azeotropically. The precipitate was filtered off and dissolved in CH2Cl2 (300 ml). The organic solution was dried, filtered and the solvent was evaporated. The residue was washed in CH3CN (50 ml), filtered off and dried, yielding 22.7 g (92%) of 2,3,4,5-tetrahydro-8-(phenyl-methoxy)-5-(phenylmethyl)-1H-pyrido[4,3-b]indole (intermediate 3).

WORKUP

后处理

  1. temperaturerefluxed for 5 hours
  2. customThe solvent was evaporated
  3. additionWater (300 ml) was added
  4. customthe organic solvent was removed azeotropically
  5. filtrationThe precipitate was filtered off
  6. dissolutiondissolved in CH2Cl2 (300 ml)
  7. customThe organic solution was dried
  8. filtrationfiltered
  9. customthe solvent was evaporated
  10. washThe residue was washed in CH3CN (50 ml)
  11. filtrationfiltered off
  12. customdried