HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 23053773, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 15620341 | HCID 15620341 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 23053773 | HCID 23053773 | — |
Reaction Steps
To 116.6 ml of dimethylformamide was added 105 ml of phosphorus oxychloride, followed by 99 g of 2-methylpyrazolo[1,5-a]pyridine under stirring at keeping the temperature below 20° C. The reaction mixture was stirred at 50°-60° C. for 1 hours, then poured into ice water. Acidic aqueous solution was neutralized with potassium carbonate, then extracted with dichloromethane, washed with salt water, dried over anhydrous sodium sulfate and then concentrated. The resulting residue was recrystallized from methanol to give the title compound in a yield of 54.8 g (46%) as colorless crystals, mp 77°-79° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04923871 |
| Source dataset | uspto-grants-1990_05 |
| ORD ID | ord-96030ff1648e481399bba50cc3765f2a |
| Source note | uspto-grants-1990_05 |