HRID1802335
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 5,6-dimethoxynicotinonitrile (1-3, 0.600 g, 3.65 mmol, 1.0 equiv) in methanol (20 mL) under a nitrogen atmosphere was added Pearlman's catalyst (0.205 g, 0.292 mmol, 0.08 equiv, 20 weight percent) and concentrated HCl (2.44 mL), and the reaction was place under an atmosphere of hydrogen. After 2 h, the reaction was placed under an atmosphere of nitrogen and filtered through celite to remove the catalyst. The reaction mixture was dissolved in EtOAc, dried over MgSO4 and concentrated to an oily solid (1-4) of high purity. ESI+MS [M+H]+ C8H12N2O2 calc'd 169.1. found 169.1.
WORKUP
后处理
- filtrationfiltered through celite
- customto remove the catalyst
- dissolutionThe reaction mixture was dissolved in EtOAc
- dry with materialdried over MgSO4
- concentrationconcentrated to an oily solid (1-4) of high purity