反応 #54764
ord-1a33f7b674034bf9ad1750ca13f03c5a
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.DISSOLUTIONwas dissolved
- 2workup.STIRRINGThe mixture was stirred at room temperature
- 3その他wrapped in foil overnight
- 4洗浄The organic layer was washed with water (3 × 100 mls.)
- 5乾燥dried over magnesium sulphate
- 6その他evaporated under vacuum
- 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%).