HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenethyl bromide → HCID 67196856, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenethyl bromide | HCID 7666 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 178499180 | HCID 178499180 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67196856 | HCID 67196856 | 31.2% |
Reaction Steps
430 mg (2.5 mM) of 4-nitro-1H-pyrazole-3-carboxylic acid methyl ester was dissolved in 4 ml of N,N-dimethylformamide, to which 0.41 ml (3 mM) of (2-bromoethyl)benzene and 1.6 g (5.0 mM) of cesium carbonate were added dropwise, and the resulting mixture was stirred under a nitrogen atmosphere for a day. The solvent was distilled off under reduced pressure, and the resultant was extracted with ethyl acetate and brine. The organic solvent layer was dried over anhydrous sodium sulfate, filtered, and then distilled under reduced pressure. The resulting impure compound was purified by column chromatography (hexane:ethyl acetate=5:1), to obtain 218 mg (31.2%) of the title compound and 506 mg (65.5%) of the compound of Preparative Example 1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939550B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-2ac6b3c378d6447c92b8f96d9b7f6aeb |
| Source note | uspto-grants-2011_05 |