반응 #1126477

ord-f57a772ff81b45bbae8215e4b9042e7a

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08552037B2uspto-grants-2013_10