HRID968607
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
Heat a solution of 5-(3-methyl(2-pyridyl))-3-nitropyridine-2-carbonitrile (1 g, 4.1 mmol), iron (2.3 g, 40 mmol) and calcium chloride (560 mg, 5 mmol) in ethanol (15 mL) and water (4 mL) to reflux for 1 hour. Cool the mixture, filter through Celite and wash with ethyl acetate. Evaporate the filtrate and re-dissolve the residue in ethyl acetate, wash with water and then with brine, dry (MgSO4) and evaporate to obtain the title compound as a pale yellow solid (880 mg, 94%).
WORKUP
后处理
- temperatureto reflux for 1 hour
- temperatureCool the mixture
- filtrationfilter through Celite
- washwash with ethyl acetate
- customEvaporate the filtrate
- dissolutionre-dissolve the residue in ethyl acetate
- washwash with water
- dry with materialwith brine, dry (MgSO4)
- customevaporate