تفاعل #427881

ord-5867e73276d34257a09adf3241cd1117

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe mixture was further stirred for 12 hr
  2. 2
    ترشيحThe reaction solution was filtered
  3. 3
    أخرىthe filtrate was evaporated under reduced pressure
  4. 4
    أخرىThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→50/50)

الإجراء التجريبي

2-Methyl-6,7-dihydro-8H-indeno[5,4-d][1,3]oxazol-8-one (1.87 g, 10.0 mmol), acetone (3.68 mL, 50.0 mmol) and ICN Alumina B (manufactured by ICN, Akt.1, 20 g) were suspended in tetrahydrofuran (50 mL), and the mixture was stirred at 50° C. for 9 hr. Acetone (3.68 mL, 50.0 mmol) was added, and the mixture was further stirred for 12 hr. The reaction solution was filtered, and the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→50/50) to give the title compound (742 mg, yield 33%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08895591B2uspto-grants-2014_11