反应详情

温度

52.5 °C

In a 10-ml round-bottomed flask, dissolve 100 mg of 4-(3H-imidazo[4,5-c]pyridin-2-yl)-fluoren-9-one, obtained in Example 1, in 3 ml of methanol, then add successively 197 mg of benzylhydrazine dihydrochloride and 138 mg of dry sodium acetate and heat at 50-55° C. for 5 hours. Pour the cooled reaction mixture into 10 ml of water, extract with ethyl acetate then twice with dichloromethane. Combine the organic phases, wash with a saturated aqueous solution of sodium chloride, dry over sodium sulphate then concentrate under reduced pressure. After purification by chromatography on silica gel (40-63 μm), eluting with a mixture of dichloromethane and methanol (93-7 by volume), we obtain 37 mg of N-benzyl-N′-[4-(1H-imidazo[4,5-c]pyridin-2-yl)-fluoren-9-ylidene]-hydrazine, in the form of a yellow foam with the following characteristics:

1. additionPour
2. extractionextract with ethyl acetate
3. washwash with a saturated aqueous solution of sodium chloride
4. dry with materialdry over sodium sulphate
5. concentrationthen concentrate under reduced pressure
6. customAfter purification by chromatography on silica gel (40-63 μm)
7. washeluting with a mixture of dichloromethane and methanol (93-7 by volume), we