Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzaldehyde | HCID 240 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Acetophenone | HCID 7410 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Product | 1H-Pyrazole, 3,5-diphenyl- | HCID 70840 | 96.5% |
Reaction Steps
60 parts (0.5 mol) of acetophenone and 53 parts (0.5 mol) of benzaldehyde were simultaneously added dropwise at 25° C. to 140 parts (1 mol) of initially introduced 70% strength by weight sulfuric acid. The mixture was stirred at 25° C. for 60 minutes and the reaction solution obtained was simultaneously added dropwise with 25 parts (0.5 mol) of hydrazine hydrate at 135° C. to 140 parts (1 mol) of initially introduced 70% strength by weight sulfuric acid and 0.5 parts (0.0033 mol)of sodium iodide in the course of 25 minutes. The mixture was stirred at 125° C. for 60 minutes. In order to keep the temperature at 135° C., 38 parts of water were distilled off. The mixture was diluted with 500 parts of water and neutralized with 247.8 parts (3.1 mol)of 50% strength by weight sodium hydroxide solution. After filtering off the solid it was washed until sulfate-free and dried. 109.7 parts of 3,5-diphenylpyrazole having a purity of 96.8% (HPLC) were obtained, which corresponds to a yield of 96.5% of theory. M.p.: 197° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05744614 |
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| Source dataset | uspto-grants-1998_04 |
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| ORD ID | ord-f1cab3c0e57c42fbbbafac9c5e7269f6 |
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| Source note | uspto-grants-1998_04 |
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