反应详情

温度

60 °C

To a suspension of 9-chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide (100 mg, 0.22 mmol) in ethanol (5 mL) add 1,8-diazabicyclo[5.4.0]undec-7-ene (40 μL, 0.27 mmol). Stir the solution under nitrogen. To the solution add (2,3-epoxypropyl)-benzene and heat to approximately 60° C. and stir under nitrogen overnight. Concentrate the reaction and dissolve in 20% isopropanol/chloroform, wash with 1N HCl, 1N sodium thiosulfate, saturated aqueous sodium bicarbonate solution, brine, dry over magnesium sulfate and concentrate. Purify by flash chromatography on silica gel (eluting with 0–1.5% methanol/chloroform) to give 85.0 mg of the title compound as a white solid, 84% yield. 1H NMR: consistent with structure. MS (ion spray) 452 (M+).

1. stirringstir under nitrogen overnight
2. concentrationConcentrate
3. customthe reaction
4. washwash with 1N HCl, 1N sodium thiosulfate, saturated aqueous sodium bicarbonate solution, brine
5. dry with materialdry over magnesium sulfate
6. concentrationconcentrate
7. customPurify by flash chromatography on silica gel (eluting with 0–1.5% methanol/chloroform)