تفاعل #304609

ord-99671a6d4e1c40538f60cbc2acc091cd

المذيبات

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe insoluble materials were removed by filtration through celite
  2. 2
    تركيزthe filtrate was concentrated under reduced pressure
  3. 3
    أخرىThe residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=95:5 to 70:30)

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08193378B2uspto-grants-2012_06