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

HRID 1198439

反応式

HRID 1198439 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-e3f1f37dee4a435092a64513ab44e627
出典データセット
uspto-grants-1994_01
特許番号
US05281592

関連ノート

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