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 mixture of 3-(1H-1,2,4-triazol-1-yl)-propanenitrile (25 g, 0.204 mol) and Raney-Nickel (5 g, 0.2 w/w, wet) in methanol (300 mL) was added a solution of 25% aqueous NH4OH (75 mL). The above reaction mixture was hydrogenated under pressure (75 psi of hydrogen) for a period of 6 h. The catalyst was then filtered off and the filtrate was concentrated under reduced pressure. The residue obtained was taken up in DCM (150 mL) then triturated 4 times and the combined organic layer was concentrated under reduced pressure to yield 22 g of the title compound as a liquid (85%). The above compound was converted to its hydrochloride using HCl gas in a mixture of ether/methanol (9.5/0.5) to yield 20 g of the product as its dihydrochloride.
WORKUP
后处理
- customThe above reaction mixture
- filtrationThe catalyst was then filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue obtained
- customthen triturated 4 times
- concentrationthe combined organic layer was concentrated under reduced pressure