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

HRID 1840351
ノート
印刷プレビュー

反応式

HRID 1840351 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

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

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,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+).

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. waitAfter 3 hours
  5. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-2c378cd1d7ed489088d99b50e2b0d845
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06680317B2

反応ノート

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