Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzylhydrazine dihydrochloride | HCID 146540 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 4-(1h-Imidazo[4,5-C]pyridin-2-Yl)fluoren-9-One | HCID 53393801 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178420368 | HCID 178420368 | 27.4% |
Reaction Steps
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:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07674795B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-cca003ae25394723b105f1054ba6c2a3 |
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| Source note | uspto-grants-2010_03 |
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