HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66918321, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 5-Chloro-2-nitrobenzaldehyde | HCID 81123 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 178498010 | HCID 178498010 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66918321 | HCID 66918321 | 53.5% |
Reaction Steps
To a solution of 4-methoxycarbonylphenylmethyltriphenylphosphine bromide (4.83 g) in THF (20 ml), potassium t-butoxide (600 mg) was added. The mixture was stirred for 1 hour at room temperature. To the reaction solution, 2-nitro-5-chlorobenzaldehyde (742 mg) was added at 0° C. The mixture was stirred for 30 minutes at room temperature. The reaction mixture was poured into diluted HCl. The mixture was extracted with hexane-AcOEt. The organic layer was washed, dried over and concentrated under the reduced pressure. The residue was purified on silica gel column chromatography (hexane-AcOEt) and recrystallization from the mixture solvent of hexane-AcOEt to give the title compound (680 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06790866B2 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-8a90218586364073854e62779b51056c |
| Source note | uspto-grants-2004_09 |