HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 89648818, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178469362 | HCID 178469362 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 89648818 | HCID 89648818 | — |
Reaction Steps
21.58 g of ethyl 1-(2-fluorobenzyl)-5-hydroxy-1H-pyrazole-3-carboxylate 1-1-2 (81.66 mmol, 1.0 eq) were dissolved in dry acetone. Then 10.17 mL of iodomethane (163.3 mmol, 2.0 eq) and 40.63 g of potassium carbonate (294 mmol, 3.6 eq) were added. The precipitate was filtered off and the filtrate was concentrated in vacuo. The residue was partitioned between DCM and water, the aqueous layer was separated and extracted with DCM twice. The combined organic layers were dried over magnesium sulfate, filtered off and concentrated in vacuo to give 14.74 g (52.96 mmol, 65%) of the crude target compound that was used for the next transformation without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422268B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-bc5541b42a11467bb891f3d29d7d0e4e |
| Source note | uspto-grants-2016_08 |