HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 67491561, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 178473417 | HCID 178473417 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 67491561 | HCID 67491561 | — |
Reaction Steps
1-Ethyl 5-methyl 3-hydroxy-1H-indazole-1,5-dicarboxylate (1.75 g, 6.62 mmol) was suspended in acetone (85 mL). Cesium carbonate (2.27 g, 6.95 mmol) and methyl iodide (1.3 mL, 20 mmol) were added and the reaction was stirred at reflux for 22 hours. The reaction was concentrated to dryness and the residue was partitioned between dichloromethane (60 mL) and water (100 mL). The layers were separated and the aqueous was extracted again with dichloromethane (60 mL). The combined organics were dried over magnesium sulfate, filtered, and concentrated. Purification by flash column chromatography (7-60% ethyl acetate/heptanes) gave two regioisomeric products.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08993586B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-ca00d240b10d484b8232445a7261e83c |
| Source note | uspto-grants-2015_03 |