反応 #54764

ord-1a33f7b674034bf9ad1750ca13f03c5a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONwas dissolved
  2. 2
    workup.STIRRINGThe mixture was stirred at room temperature
  3. 3
    その他wrapped in foil overnight
  4. 4
    洗浄The organic layer was washed with water (3 × 100 mls.)
  5. 5
    乾燥dried over magnesium sulphate
  6. 6
    その他evaporated under vacuum
  7. 7
    その他The product was recrystallised from ethyl acetate/hexane

実験手順

2(4-Chlorobutyramido)-4-methyloxazole (2.20 g., 0.018 mol) prepared as described in Example 36 was dissolved with stirring under nitrogen in dry benzene (350 mls.) and 1:5-diazobicyclo[4,3,0]non-5-ene (1.47 g., 0.0118 mol) in dry benzene (50 mls.) was added with stirring over 10 minutes. The mixture was stirred at room temperature, wrapped in foil overnight. The organic layer was washed with water (3 × 100 mls.) dried over magnesium sulphate and evaporated under vacuum. The product was recrystallised from ethyl acetate/hexane. WT.= 0.75 g. m.p. 116° C. (Yield = 41.57%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04150143uspto-grants-1979_04