反応 #346354

ord-13912584cd0d47cd8a0335c54d569d09

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度while cooling in an ice bath
  3. 3
    workup.STIRRINGThe mixture was stirred for 3 hours
  4. 4
    ろ過The precipitate was collected by filtration
  5. 5
    洗浄washed with water
  6. 6
    その他dried

実験手順

2,2,2-trichloroethyl 6-(2-phenylacetamido)-2,2-dimethylpenam-3-carboxylate (466 mg.) was added to acetic acid (2 cc), and sodium percarbonate (377 mg.) was added thereto while cooling in an ice bath. The mixture was stirred for 30 minutes, and sodium tungstate dihydrate (40 mg.), acetic acid (1 cc) and water (1 cc) were added thereto. The mixture was stirred for 3 hours, and then water (50 cc) was added thereto. The precipitate was collected by filtration, washed with water and dried to yield crude crystals (400 mg.) of 2,2,2-trichloroethyl 6-(2-phenylacetamido)-2,2-dimethylpenam-3-carboxylate-1-oxide, m.p. 165° - 167° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04036847uspto-grants-1977_07