HRID2108194
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationAfter complete hydrogenation, the catalyst was filtered off Most of the solvent
- customwas evaporated
- extractionextracted with ether
- dry with materialThe ether-phase was dried (Na2SO4)
- customthe solvent evaporated