Reaktion #304609
ord-99671a6d4e1c40538f60cbc2acc091cd
Reaktionsgleichung
EtOAc
K2CO3
2-hydroxy-4-(methoxymethoxy)benzaldehyde
3-methyl 2-butanal
→
7-(methoxymethoxy)-2,2-dimethyl-2H-chromene-3-carbaldehyde
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigethe insoluble materials were removed by filtration through celite
- 2Einengenthe filtrate was concentrated under reduced pressure
- 3SonstigeThe residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=95:5 to 70:30)
Vorschrift
K2CO3 (835 mg) was suspended in dioxane (40 mL), and 2-hydroxy-4-(methoxymethoxy)benzaldehyde (1 g) and 3-methyl 2-butanal (0.787 mL) were added thereto, followed by stirring at 110° C. overnight. EtOAc was added thereto, the insoluble materials were removed by filtration through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=95:5 to 70:30) to obtain 7-(methoxymethoxy)-2,2-dimethyl-2H-chromene-3-carbaldehyde (320 mg) as a yellow oil.