HRID1603731

反应详情

EQUATION

反应方程式

HRID 1603731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-bromomethyl-1,2,3,4-tetrahydronaphthalene (1.33 g, 5.91 mmol) and 4-methoxyphenethylamine (1.79 g, 11.8 mmol) in 50 ml of EtOH was refluxed for 48 hours. After removal of EtOH in vacuo, the residue was dissolved in 100 ml of CHCl3, washed with 10% K2CO3, H2O, sat'd brine, and then dried over Na2SO4. Filtration followed by evaporation of solvent gave a yellow oil, which was purified by chromatography (SiO2, MeOH:CHCl3, 5:95) to a give a yellowish oil (1.03 g, 58.9%). The product was converted to HCl salt, crystallization with MeOH/Et2O gave a white powder. mp 274-275° C..; Calcd for C20H25NO.HCl: C 72.37, H 7.91, N 4.22; Found C 72.40, H 7.76, N 4.13.

WORKUP

后处理

  1. customAfter removal of EtOH in vacuo
  2. dissolutionthe residue was dissolved in 100 ml of CHCl3
  3. washwashed with 10% K2CO3, H2O
  4. dry with materialdried over Na2SO4
  5. filtrationFiltration
  6. customfollowed by evaporation of solvent
  7. customgave a yellow oil, which
  8. customwas purified by chromatography (SiO2, MeOH:CHCl3, 5:95) to