N-Methyl-6-chloro-2-hydroxy-3-nitrobenzenesulfonamide → N-Methyl-3-amino-6-chloro-2-hydroxybenzenesulfonamide

HRID 2301505노트

반응식

HRID 2301505 반응식
[CH3:1][NH:2][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][NH:2][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]

참가 물질

4

반응물 1

HCID 18373432N-Methyl-6-chloro-2-hydroxy-3-nitrobenzenesulfonamide

생성물 1

HCID 18373530N-Methyl-3-amino-6-chloro-2-hydroxybenzenesulfonamide수율 127.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of N-methyl-6-chloro-2-hydroxy-3-nitrobenzenesulfonamide (140 mg, 0.53 mmol) in ethyl acetate, was added 10% Pd/C (60 mg). The mixture was flushed with argon, then stirred under a hydrogen atmosphere at balloon pressure for 1.5 hours at room temperature. The mixture was filtered through celite and the celite was washed with methanol. The solvent was evaporated to give the desired product (160 mg, >100%). 1H NMR (DMSO-d6): δ 7.95 (bs, 1H), 6.85 (d, 1H), 6.79 (d, 1H), 2.48 (d, 3H).

후처리

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

출처 및 근거

ORD 기록
ord-c105672e4e834c46af0a78c49699078a
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06500863B1

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