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

HRID 2301505ノート

反応式

HRID 2301505 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c105672e4e834c46af0a78c49699078a
出典データセット
uspto-grants-2002_12
特許番号
US06500863B1

反応ノート

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