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N,N-Dimethyl-6-chloro-2-hydroxy-3-nitrobenzenesulfonamide → N,N-Dimethyl-3-amino-6-chloro-2-hydroxybenzenesulfonamide

HRID 1840351
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HRID 1840351 반응식
[CH3:1][N:2]([CH3:17])[S:3]([C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[C:8]([N+:13]([O-])=O)[C:7]=1[OH:16])(=[O:5])=[O:4]>C(OCC)(=O)C.[Pd]>[CH3:1][N:2]([CH3:17])[S:3]([C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[C:8]([NH2:13])[C:7]=1[OH:16])(=[O:5])=[O:4]
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참가 물질

4

반응물 1

HCID 23447760N,N-Dimethyl-6-chloro-2-hydroxy-3-nitrobenzenesulfonamide

생성물 1

HCID 23447758N,N-Dimethyl-3-amino-6-chloro-2-hydroxybenzenesulfonamide수율 98%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of N,N-Dimethyl-6-chloro-2-hydroxy-3-nitrobenzenesulfonamide (550 mg, 1.96 mmol) in ethyl acetate, was added 10% Pd/C (550 mg). The mixture was flushed with argon, and then stirred under a hydrogen atmosphere at balloon pressure for 3 hours at room temperature. TLC showed the reaction was not complete. The mixture was filtered through celite and the celite was washed with methanol. The mixture was retreated under the same conditions as mentioned above. After 3 hours, the solvent was evaporated to give the desired product (480 mg, 98%). EI-MS (m/z) 250.82, 252.87 (M+).

후처리

  1. customThe mixture was flushed with argon
  2. filtrationThe mixture was filtered through celite
  3. washthe celite was washed with methanol
  4. waitAfter 3 hours
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-2c378cd1d7ed489088d99b50e2b0d845
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06680317B2

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