HRID1953414
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 2-[3-[(E)-2-[5-[(E)-2-(4-pyridyl)vinyl]pyridin-3-yl]vinyl]phenylamino]-3-nitropyridine (331 mg), iron powder (132 mg) and ammonium formate (297 mg) in ethanol (6 ml) and water (2 ml) was stirred at 90pbC. for 30 minutes. The mixture was filtered while hot. The filtrate was added to aqueous sodium bicarbonate solution and extracted with ethyl acetate twice. The combined organic solution was washed with sodium bicarbonate and brine, dried over magnesium sulfate and concentrated. The resultant solid was washed with diisopropyl ether to give 3-amino-2-[3-[(E)-2-[5-[(E)-2-(4-pyridyl)vinyl]pyridin-3-yl]vinyl]phenylamino]pyridine (270 mg).
WORKUP
后处理
- filtrationThe mixture was filtered while hot
- additionThe filtrate was added to aqueous sodium bicarbonate solution
- extractionextracted with ethyl acetate twice
- washThe combined organic solution was washed with sodium bicarbonate and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- washThe resultant solid was washed with diisopropyl ether