HRID2194791
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
3-Bromomethyl-4-chloro-5-methyl-benzonitrile (0.9938 g, 4.06 mmol), potassium cyanide (0.529 g, 8.12 mmol) in ethanol (5.0 mL) and H2O (2.5 mL) was heated at 85° C. for 3 hr. The reaction mixture was cooled, diluted with ethyl acetate, washed with brine, dried (MgSO4), concentrated and purified by flash column chromatography (silica gel, 0 to 30% ethyl acetate/hexane) to give 4-chloro-3-cyanomethyl-5-methyl-benzonitrile as a white solid (0.3707 g, 48%). 1H NMR (300 MHz, CDCl3): 7.61 (s, 1H), 7.51 (s, 1H), 3.83 (s, 2H), 2.40 (s, 3H).
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- washwashed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
- custompurified by flash column chromatography (silica gel, 0 to 30% ethyl acetate/hexane)