Ammonium Hydroxide → 3-Chloro-4-fluorobenzenesulfonamide

HRID 396805ノート

反応式

HRID 396805 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].[OH-].[NH4+:14]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([NH2:14])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8]

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 1452223-Chloro-4-fluorobenzenesulphonyl chloride

生成物 1

HCID 75098833-Chloro-4-fluorobenzenesulfonamide収率 68.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-chloro-4-fluorobenzenesulfonyl chloride (2.29 g, 10 mmol) in methylene chloride (30 mL) was added 25% ammonium hydroxide (10 mL) at room temperature and the mixture was stirred for 1 hour. The solvent was removed in vacuo. The residue was redissolved in ethyl acetate (50 mL) and the whole washed with water and brine. After dried over MgSO4 and concentration in vacuo. The resulting solid was recrystallized from ether-hexane to give the title compound (1.429 g, 68.2% yield).

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionThe residue was redissolved in ethyl acetate (50 mL)
  3. washthe whole washed with water and brine
  4. dry with materialAfter dried over MgSO4 and concentration in vacuo
  5. customThe resulting solid was recrystallized from ether-hexane

出典と根拠

ORDレコード
ord-35ed3c7eae97476587ee23a525a81a07
出典データセット
uspto-grants-2003_08
特許番号
US06608095B2

反応ノート

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