반응 #5923

ord-8a5b4bf891e840f68c2652294c346d36

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The ethyl acetate layer is washed
  2. 2
    기타dried
  3. 3
    workup.DISTILLATIONdistilled
  4. 4
    기타to remove the solvent
  5. 5
    기타The residue is recrystallized from ethyl acetate-n-hexane

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246929uspto-grants-1993_09