HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → 5-azidocarbonyl-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 5-(Methoxycarbonyl)-1-Methyl-1H-Pyrazole-3-Carboxylic Acid | HCID 14266056 | — |
| Solvent | Water | HCID 962 | — |
| Product | 5-azidocarbonyl-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester | HCID 57619362 | — |
Reaction Steps
1-Methyl-1H-pyrazole-3,5-dicarboxylic acid 5-methyl ester (641, 3.2 g, 17.0 mmol) was combined with thionyl chloride (5 mL). The reaction was heated to reflux for 40 minutes and then concentrated twice from toluene. The resulting solid was dried under reduced pressure overnight. The product was dissolved into acetone (20 mL) and sodium azide (3.5 g, 54.0 mmol) was added in water (10 mL) rapidly at once. The obtained solution was stirred for one minute and then poured into ice-water (50 mL). The precipitate was filtered and dried under reduced pressure. The final compound was used without further purification (642, 2.8 g, 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169250B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-246b01c2b97c4ea3962bb2ed17c830c0 |
| Source note | uspto-grants-2015_10 |