HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → ethyl 1-isopropyl-1H-pyrazole-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Isopropyl iodide | HCID 6362 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | HCID 178469268 | HCID 178469268 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | ethyl 1-isopropyl-1H-pyrazole-3-carboxylate | HCID 23005998 | 96% |
Reaction Steps
To 1H-pyrazole-3-carboxylic acid ethyl ester (23.1 g, 165 mmol) in THF (330 mL) was added 2-iodopropane (33.0 mL, 330 mmol) followed by NaOEt (21% in EtOH, 65.0 mL, 174 mmol). This solution was then heated to reflux for 16 h. The reaction was then allowed to cool to room temperature. AcOH (10.5 mL, 183 mmol) was added and the reaction was stirred for 5 min. H2O (400 mL) was added to the solution, and this mixture was extracted with EtOAc (3×150 mL). The combined organic was washed with sat. aq. NaHCO3, then brine. The organic was dried over MgSO4, filtered, and concentrated to give the product (28.70 g, 96%) as a brown oil containing a 98:2 mixture of regioisomers by 1H NMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853202B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-745281b5643741f2b75cd2e3cf769d82 |
| Source note | uspto-grants-2014_10 |