反応 #54762

ord-07097c77bf794604bc3b2c694c5a8945

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe mixture was stirred for a further 2 hours at room temperature
  2. 2
    workup.ADDITIONpoured onto ice-water (250 ml.)
  3. 3
    抽出extracted with ether (3 × 100 ml.)
  4. 4
    洗浄The extract was washed with dilute hydrochloric acid
  5. 5
    乾燥with sodium chloride solution, dried over sodium sulphate
  6. 6
    その他evaporated
  7. 7
    workup.DISTILLATIONThe residue was distilled under vacuum

実験手順

Sodium hydride (2.8 g. of a 50% dispersion in oil, 0.058 mol) was added in small portions to a stirred solution of 2-(2-ethylbutyramido)-4-methyloxazole (8.0 g., 0.041 mol) in dimethylformamide (100 ml.) at -5° to 0° C. The mixture was stirred for 2 hours at room temperature and then ethyl iodide (4.7 ml. 0.058 mol) was added. The mixture was stirred for a further 2 hours at room temperature and then poured onto ice-water (250 ml.) and extracted with ether (3 × 100 ml.). The extract was washed with dilute hydrochloric acid, then with sodium chloride solution, dried over sodium sulphate and evaporated. The residue was distilled under vacuum to give the product 4.7 g. (51%) b.p. 71-72° C/0.3 mm.

出典

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