反応 #5923

ord-8a5b4bf891e840f68c2652294c346d36

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The ethyl acetate layer is washed
  2. 2
    その他dried
  3. 3
    workup.DISTILLATIONdistilled
  4. 4
    その他to remove the solvent
  5. 5
    その他The residue is recrystallized from ethyl acetate-n-hexane

実験手順

To a mixture of 2-(4-chlorophenyl)-3,4-dihydro2H-1,4-benzothiazine (1.08 g), ethyl acetate (20 ml) and aqueous sodium hydrogen carbonate solution (20 ml) is added dropwise a solution of 4-bromobutyryl chloride (0.97 g) in ethyl acetate (5 ml) with stirring under ice cooling. The ethyl acetate layer is washed, dried and distilled to remove the solvent. The residue is recrystallized from ethyl acetate-n-hexane to give 4-(4-bromobutyryl)-2-(4-chlorophenyl)-3,4-dihyro-2H-1,4-benzothiazine (1.58 g, yield 93%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246929uspto-grants-1993_09