HRID626764
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 suspension of [1-(4-azido-5-fluoropyridin-3-yl)-meth-(E)-ylidene]-(2,6-dichloro-4-nitrophenyl)-amine (5.89 g, 16.6 mmol) in toluene (80 mL) was heated at 105° C. for 4 hours. The resultant mixture was cooled to room temperature and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (0-5% methanol in DCM) to afford the title compound (4.78 g, 81% yield). 1H NMR (300 MHz, CDCl3): δ 9.13 (d, J=2.2 Hz, 1H), 8.43 (s, 2H), 8.39 (d, J=2.4 Hz, 1H), 8.26 (d, J=3.4 Hz, 1H).
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel flash chromatography (0-5% methanol in DCM)