反应详情

温度

70 °C

To a mixture of 300 mg of (0.884 mmol) 8-chloro-1-(2-chloro-phenyl)-1H-imidazo[4,5-c]quinoline-2-carbonitrile (Example 84) and 245 mg (3.537 mmol) hydroxylamine hydrochloride in 7.5 ml DMF, a solution of 326 mg (3.08 mmol) sodium carbonate in 1.8 ml water is added by syringe within 2 min. The reaction mixture is heated at 70° C. for 4½ h. The cold solution is poured in ice-water and stirred for 1 h. The precipitate which is formed is filtered off and washed with water and ethanol. The compound is dried over night at 60° C. (high vacuum). mp: 265-267° C.; MS: 372 (M++1); HPLC: tret=80.43 min (Grad 1).

1. customThe precipitate which is formed
2. filtrationis filtered off
3. washwashed with water and ethanol
4. customThe compound is dried over night at 60° C. (high vacuum)
5. customtret=80.43 min (Grad 1)