HRID626754
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
A solution of 2-{[1-(4-azido-5-fluoropyridin-3-yl)-meth-(E)-ylidene]-amino}-3-chlorobenzonitrile (5.16 g, 17.2 mmol) in toluene (60 mL) was heated at 105° C. for 5 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 as a beige solid (2.57 g, 55% yield). 1H NMR (400 MHz, DMSO-d6): δ 9.42 (d, J=2.6 Hz, 1H), 9.26 (d, J=2.5 Hz, 1H), 8.33 (d, J=3.8 Hz, 1H), 8.24-8.19 (m, 2H), 7.92 (t, J=8.1 Hz, 1H).
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel flash chromatography (0-5% methanol in DCM)