HRID2108194

反应详情

EQUATION

反应方程式

HRID 2108194 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(3-pyridinyl)methoxybenzene (22.0 g, 0.099 mol) in methanol (250 ml), PtO2 (2 g) and conc. HCl (30 ml) were added and the mixture was hydrogenated at 0.34 MPa in a Parr apparatus. After complete hydrogenation, the catalyst was filtered off Most of the solvent was evaporated, the residue was made alkaline with 1M NaOH and extracted with ether. The ether-phase was dried (Na2SO4) and the solvent evaporated giving 18 g of the amine product. The hydrochloride was made and then recrystallized from ethanol/ether yielding 20.9 g (93%), mp. 137-138.5° C.

WORKUP

后处理

  1. filtrationAfter complete hydrogenation, the catalyst was filtered off Most of the solvent
  2. customwas evaporated
  3. extractionextracted with ether
  4. dry with materialThe ether-phase was dried (Na2SO4)
  5. customthe solvent evaporated