HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chlorobenzaldehyde → HCID 178468899, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chlorobenzaldehyde | HCID 6996 | — |
| Reactant | Ethyl isobutyrylacetate | HCID 81583 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 178418806 | HCID 178418806 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178468899 | HCID 178468899 | 3.3% |
Reaction Steps
2-Chlorobenzaldehyde (1.41 g), 3-aminopyrazole (0.83 g) and ethyl isobutyrylacetate (1.58 g) were stirred in acetic acid (10 ml) at 80° C. for 2 hours. Under ice-cooling, a saturated aqueous sodium hydrogencarbonate solution was added to the reaction mixture. The insoluble material was filtered off, and the mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The extract was concentrated under reduced pressure and the obtained residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1)). The purified product was crystallized from hexane-ethyl acetate to give the title compound (115 mg) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06977262B2 |
| Source dataset | uspto-grants-2005_12 |
| ORD ID | ord-4af1c7d3360c4cfdb4837ec992dacc55 |
| Source note | uspto-grants-2005_12 |