HRID1522573
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
To a solution of 2-(3-fluoro-6-methylpyridin-2-yl)-5-methyl-4-nitropyridine 1-oxide (2.7 g, 10.2 mmol) in AcOH (54 mL) was added iron (2.3 g, 40.9 mmol) and the mixture was stirred at 100° C. for 30 minutes, cooled to room temperature, adjusted pH to about 8 with NaOH (1N) and extracted with ethyl acetate. The organic layers were concentrated to give 3′-fluoro-5,6′-dimethyl-2,2′-bipyridin-4-amine. 1HNMR (CDCL3) δ ppm 8.32 (s, 1H), 7.43-7.38 (m, 1H), 7.19-7.15 (m, 2H), 4.19 (s, 2H), 2.65 (s, 3H), 2.19 (s, 3H). MS [M+H] found 218.0.
WORKUP
后处理
- temperaturecooled to room temperature
- extractionextracted with ethyl acetate
- concentrationThe organic layers were concentrated