Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | 4-Chlorobenzaldehyde | HCID 7726 | — |
| Reactant | p-METHYLACETOPHENONE | HCID 8500 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Product | HCID 11737273 | HCID 11737273 | 92% |
Reaction Steps
326.7 parts (2 mol) of sulfuric acid were initiially introduced into the stirring flask. 37.5 parts (0.75 mol) of hydrazine hydrate, 100 parts (0.75 mol) of 4-methylacetophenone, 105 parts (0.75 mol) of 4-chlorobenzaldehyde and 1 part (0.0067 mol) of sodium iodide were meteredin in succession at room temperature. The reaction mixture was brought to 140° C. by distilling off water and kept at 140° C. for 2.5 hours. 140 parts of water were distilled off. The mixture was diluted with500 parts of water and neutralized with 500 parts (12.5 mol) of 20% strength by weight sodium hydroxide solution. After filtering off the solid it was washed until sulfate-free and dried. 189 parts of 3-(4-chlorophenyl)-5-(4-methylphenyl)pyrazole having a purity of 98% (HPLC) were obtained, which corresponds to a yield of 92% of theory. M.p.:228° 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-a1bff667685b4c83a9ea42ef0e1c7649 |
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| Source note | uspto-grants-1998_04 |
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