HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 85968314, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4-nitro-1H-pyrazole | HCID 16376 | — |
| Reactant | 2,2-Dimethyl-1,3-dioxolan-4-ylmethyl p-toluenesulfonate | HCID 235097 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 85968314 | HCID 85968314 | 88.9% |
Reaction Steps
A solution of (2,2-dimethyl-1,3-dioxolan-4-yl)methyl 4-methylbenzenesulfonate (1.57 g, 5.5 mmol), 4-nitro-1H-pyrazole (0.57 g, 5.0 mmol) and cesium carbonate (4.89 g, 15.0 mmol) in acetonitrile (30 mL) was stirred at 70° C. under N2 overnight. The reaction mixture was filtered, and the resulting filtrate was concentrated. The residue was diluted with ethyl acetate (50 mL), washed with water (50 mL×2) and brine (50 mL), dried over sodium sulfate, filtered, and concentrated to afford 1-((2,2-dimethyl-1,3-dioxolan-4-yl)methyl)-4-nitro-1H-pyrazole (1.01 g, crude), which was directly used in the next step without further purification. MS (ES+) C9H13N3O4 requires: 227, found: 228 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09334263B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-705035faee5744e1a7c1e397102c5917 |
| Source note | uspto-grants-2016_05 |