Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 2',4'-Dihydroxyacetophenone | HCID 6990 | — |
| Reactant | 2-Hydrazinopyridine | HCID 78645 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136365341 | HCID 136365341 | 50% |
Reaction Steps
A total of 33.8 g (0.309 mol) of 2-hydrazinopyridine and 2 L of methanol were charged into a four-neck flask with a capacity of 3 L equipped with a reflux condenser, a thermometer, and a stirrer, and 1 mL of concentrated sulfuric acid was then dropwise added at room temperature under stirring. Then, 44.0 g (0.289 mol) of 2,4-dihydroxyacetophenone was charged and a reaction was conducted for 8 h at 40° C. under stirring. The precipitated crystals were taken out by filtration, washed with methanol and water and dried at 60° C. to obtain 33.0 g of 4-{1-[(2-pyridine-2-yl)hydrazono]ethyl}benzene-1,3-diol in the form of light-yellow crystals. The yield was 50%. GC/MS, 1H-NMR, and IR measurements were performed with respect to the obtained crystals. The results are shown below.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07951903B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-da77ba841e2d4fe992ecf1a74b3e5517 |
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| Source note | uspto-grants-2011_05 |
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