Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phenylhydrazine | HCID 7516 | — |
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,8-Dimethylnonane-4,6-dione | HCID 581379 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 20542766 | HCID 20542766 | 44% |
Reaction Steps
10 grams diisovalerylmethane (as described by Swamer and Hauser), were reacted with 1.3 gram of a 50% suspension of sodium hydride in paraffin oil and 10 grams bromoacetic acid-ethylester by a procedure analogous to that described in Example (2b). The benzene solution obtained in this procedure was evaporated and the residue of crude 3,3-diisovalerylpropionic acid-ethyl ester obtained thereby was mixed with 6.5 grams phenylhydrazine and 4 grams glacial acetic acid and the mixture was heated to the boiling temperature under reflux for 2 hours. The reaction mixture obtained thereby was then worked up in accordance with a procedure analogous to that described in Example (1a). The ester thus recovered was saponified and the free acid recovered by a procedure analogous to that described in Example (1b). 7.5 grams 3,5-diisobutyl-1-phenyl-pyrazol-4-acetic acid, melting at 125°-126° C., were obtained representing a yield of 44% on the diisovalerylmethane starting material.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04325962 |
|---|
| Source dataset | uspto-grants-1982_04 |
|---|
| ORD ID | ord-1a7d8813803d4d13a8a301ae558ab689 |
|---|
| Source note | uspto-grants-1982_04 |
|---|