Hydrazinium hydrate → 4-(4-Aminobenzylamino)-N-(4,6-dimethylpyrimidin-2-yl)-benzenesulfonamide

HRID 1884825

反応式

HRID 1884825 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH:9][S:10]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][C:21]3[CH:26]=[CH:25][C:24]([N+:27]([O-])=O)=[CH:23][CH:22]=3)=[CH:15][CH:14]=2)(=[O:12])=[O:11])[N:3]=1.O.[NH3+]N>O1CCCC1.[Pd]>[NH2:27][C:24]1[CH:25]=[CH:26][C:21]([CH2:20][NH:19][C:16]2[CH:15]=[CH:14][C:13]([S:10]([NH:9][C:4]3[N:3]=[C:2]([CH3:1])[CH:7]=[C:6]([CH3:8])[N:5]=3)(=[O:12])=[O:11])=[CH:18][CH:17]=2)=[CH:22][CH:23]=1

参加物

5

反応物 2

HCID 22629909Hydrazinium hydrateHCID 23504906N-(4,6-dimethylpyrimidin-2-yl)-4-(4-nitrobenzylamino)-benzenesulfonamide

生成物 1

HCID 235048974-(4-Aminobenzylamino)-N-(4,6-dimethylpyrimidin-2-yl)-benzenesulfonamide収率 59%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

18 mg (0.04 mmol) of N-(4,6-dimethylpyrimidin-2-yl)-4-(4-nitrobenzylamino)-benzenesulfonamide was dissolved in 1 ml of tetrahydrofurane. Hydrazinium hydrate (50 μl, 1.5 mmol) and catalytic amount of palladium on charcoal were added to the reaction mixture. Solution was stirred overnight. The reaction mixture was evaporated to dryness and purified on silica using gradient elution (chloroform to 4% methanol in chloroform) to obtain with a yield of 59%. MS (ESI+): m/z 406 (M+H)+, 384 (M+H)+.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. custompurified on silica using gradient elution (chloroform to 4% methanol in chloroform)
  3. customto obtain with a yield of 59%

出典と根拠

ORDレコード
ord-c130c63bdc8745a4871f6c1c72ea3508
出典データセット
uspto-grants-2004_07
特許番号
US06767909B2

関連ノート

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