HRID931167
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
A solution of 5-(chloromethyl)-1-methyl-1H-1,2,4-triazole hydrochloride (1.5 g, 11.45 mmol) in dimethylsulfoxide (30 mL) was added to a stirred suspension of sodium cyanide (3.366 g, 68.70 mmol) in dimethylsulfoxide (20 mL), and the reaction mixture was stirred at room temperature for 16 h. The mixture was partitioned between ethyl acetate and water. The organic layer was dried over sodium sulfate and concentrated. The resulting crude product was purified via column chromatography (100-200 mesh silica gel, 10-12% ethyl acetate in petroleum ether) to afford 2-(1-methyl-1H-1,2,4-triazol-5-yl)acetonitrile (1.2 g). MS (ES+APCI) (M+H) 123.2.
WORKUP
后处理
- customThe mixture was partitioned between ethyl acetate and water
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated
- customThe resulting crude product was purified via column chromatography (100-200 mesh silica gel, 10-12% ethyl acetate in petroleum ether)