HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Formic Acid → 6-Bromo-4,4-dimethyl-3,4-dihydroquinoline-1(2H)-carbaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Formic Acid | HCID 284 | — |
| Edukt | 6-Bromo-1,2,3,4-tetrahydro-4,4-dimethylquinoline | HCID 10823932 | — |
| Produkt | 6-Bromo-4,4-dimethyl-3,4-dihydroquinoline-1(2H)-carbaldehyde | HCID 22568883 | 90% |
Reaktionsschritte
A solution of 6-bromo-4,4-dimethyl-1,2,3,4-tetrahydroquinoline, available in accordance with U.S. Pat. No. 5,089,509, the specification of which is incorporated herein by reference (1.8 g, 7.5 mmol) in 10 mL of formic acid was refluxed for 3 h. The reaction mixture was then cooled to ambient temperature and poured into ice-cold saturated aqueous sodium bicarbonate solution and extracted with diethyl ether (×2). The combined organic phase was dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to a residue which was subjected to flash column chromatography over silica gel (230-400 mesh) using 15-25% ethyl acetate in hexane as the eluent to afford the title compound as a pale yellow solid (1.8 g, 90%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06713647B2 |
| Quelldatensatz | uspto-grants-2004_03 |
| ORD ID | ord-d12bcbc79f4040ac830becd35f324354 |
| Quellennotiz | uspto-grants-2004_03 |