2,5-Dichlorobenzenesulfonamide → 2-Mercapto-5-Chloro-benzenesulfonamide

HRID 3693ノート

反応式

HRID 3693 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[S:9]([NH2:12])(=[O:11])=[O:10].[SH2:13].[Na]>CN(C=O)C>[SH:13][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[S:9]([NH2:12])(=[O:11])=[O:10]

参加物

4

反応物 2

HCID 2380452,5-DichlorobenzenesulfonamideHCID 86586439Sodium hydrogen sulphide

生成物 1

HCID 189353412-Mercapto-5-Chloro-benzenesulfonamide収率 30.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 34.0 g (0.15 mol) of 2,5-dichloro-benzene sulfonamide in 200 mL of DMF was added 16.0 g (0.28 mol) of sodium hydrogensulfide. The mixture was refluxed for 18 hours, then cooled, concentrated, and the solids collected by filtration. The solids were dissolved in hot water, the pH adjusted to 4.0 and the precipitate filtered. This material was dried to yield 10.1 g of the title compound, mp 142°-144° C.

後処理

  1. temperatureThe mixture was refluxed for 18 hours
  2. temperaturecooled
  3. concentrationconcentrated
  4. filtrationthe solids collected by filtration
  5. dissolutionThe solids were dissolved in hot water
  6. filtrationthe precipitate filtered
  7. customThis material was dried

出典と根拠

ORDレコード
ord-18a0ff4af7384269a935d5430d7f8ca8
出典データセット
uspto-grants-1998_03
特許番号
US05734081

反応ノート

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