HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 58764244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Hexamethylphosphoramide | HCID 12679 | — |
| Reactant | 5-Chloro-1,3-dimethylpyrazole-4-carboxaldehyde | HCID 2777397 | — |
| Reactant | 1,4-Oxazepane hydrochloride | HCID 23090214 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58764244 | HCID 58764244 | 61.2% |
Reaction Steps
Homomorpholine hydrochloride (28.2 g, 200 mol) was added to a mixture of 5-chloro-1,3-dimethyl-1H-pyrazole-4-carbaldehyde (21.68 g, 0.1368 mol, Example B(45), Step 2), HMPA (30 mL), water (50 mL), and potassium carbonate (59 g, 0.6 mol) at constant stirring and room temperature. The reaction mixture was heated at 80° C. for 50 h, diluted with water, and extracted with ethyl acetate (3×100 mL). The organic extracts were washed with water to weakly alkaline pH and dried with sodium sulfate. The product was purified chromatographically using hexane/ethyl acetate mixture as eluent to afford the title product (18.7 g, 61%). Satisfactory C,H,N-analysis was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07151105B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-19ef3d7858a740db8a08da910325983f |
| Source note | uspto-grants-2006_12 |