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

HRID 3693노트

반응식

HRID 3693 반응식
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]

참가 물질

4

반응물 2

HCID 2380452,5-DichlorobenzenesulfonamideHCID 86586439Sodium hydrogen sulphide

생성물 1

HCID 189353412-Mercapto-5-Chloro-benzenesulfonamide수율 30.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-18a0ff4af7384269a935d5430d7f8ca8
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05734081

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