HRID626700
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
- 105 °C
PROCEDURE
实验过程
A mixture of [1-(4-azidopyridin-3-yl)meth-(E)-ylidene]-(2,6-dichloro-4-fluorophenyl)amine (2.09 g, 6.75 mmol) in toluene (20 mL) was heated to 105° C. for 45 minutes. The reaction was cooled and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (50-100% ethyl acetate in cyclohexane) to afford the title compound as a yellow solid (1.60 g, 84% yield). 1H NMR (300 MHz, CDCl3): δ 9.38 (s, 1H), 8.45-8.30 (m, 2H), 7.70 (d, J=6.5 Hz, 1H), 7.32 (d, J=7.7 Hz, 2H).
WORKUP
后处理
- temperatureThe reaction was cooled
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel flash chromatography (50-100% ethyl acetate in cyclohexane)