4-Bromobutyryl chloride → 4-(4-bromobutyryl)-2-(4-chlorophenyl)-3,4-dihyro-2H-1,4-benzothiazine

HRID 1198439

반응식

HRID 1198439 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][NH:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[S:9]2)=[CH:4][CH:3]=1.C(=O)([O-])O.[Na+].[Br:23][CH2:24][CH2:25][CH2:26][C:27](Cl)=[O:28]>C(OCC)(=O)C>[Br:23][CH2:24][CH2:25][CH2:26][C:27]([N:12]1[C:11]2[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=2[S:9][CH:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[CH2:13]1)=[O:28]

참가 물질

5

반응물 3

HCID 702254-Bromobutyryl chlorideHCID 516892Sodium BicarbonateHCID 130715242-(4-chlorophenyl)-3,4-dihydro2H-1,4-benzothiazine

생성물 1

HCID 700447724-(4-bromobutyryl)-2-(4-chlorophenyl)-3,4-dihyro-2H-1,4-benzothiazine수율 93.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a mixture of 2-(4-chlorophenyl)-3,4-dihydro-2H-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%).

후처리

  1. washThe ethyl acetate layer is washed
  2. customdried
  3. distillationdistilled
  4. customto remove the solvent
  5. customThe residue is recrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-e3f1f37dee4a435092a64513ab44e627
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05281592

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