HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 22281967, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1-Acetoxy-2-bromoethane | HCID 13564 | — |
| Reactant | HCID 178423894 | HCID 178423894 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22281967 | HCID 22281967 | 12.7% |
Reaction Steps
To 3-amino-1-methyl-4-(4-methylphenyl)-1H-pyrazol-5-ol (Preparation 3b) (855 mg) in dimethylformamide (10 ml) at room temperature was added cesium carbonate (4.11 g) and 2-bromoethyl acetate (703 mg), the mixture was stirred for 45 minutes. The reaction was diluted with 2M hydrochloric acid (10 ml) and extracted with ether (2×100 ml). The organic fractions were combined, washed with water (2×100 ml) and brine (100 ml), dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (silica, 30 g) eluted with ethyl acetate:hexane (5:1) to yield the title compound as a white solid (155 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06573270B1 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-9c2e68ccb81f45d6a6be90310a619d54 |
| Source note | uspto-grants-2003_06 |