Hydrazine hydrate (1:1) → 4-((3-amino-1H-1,2,4-triazol-5-yl)amino)benzenesulfonamide

HRID 1179262ノート

反応式

HRID 1179262 の反応式
[C:1]([N:3]=[C:4](OC1C=CC=CC=1)[NH:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([NH2:15])(=O)=[O:13])=[CH:8][CH:7]=1)#[N:2].[OH2:23].[NH2:24][NH2:25]>>[NH2:2][C:1]1[NH:25][N:24]=[C:4]([NH:5][C:6]2[CH:7]=[CH:8][C:9]([S:12]([NH2:15])(=[O:13])=[O:23])=[CH:10][CH:11]=2)[N:3]=1

参加物

3

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 178512286phenyl N'-cyano-N-(4-sulfamoylphenyl)carbamimidate

生成物 1

HCID 113797954-((3-amino-1H-1,2,4-triazol-5-yl)amino)benzenesulfonamide収率 87.4%

反応条件

温度
70 °C

実験手順

To a solution of 4-(3-cyano-2-phenyl-isoureido)-benzenesulfonamide (1.35 mmol) in TBF (5 ml), was added a solution of hydrazine monohydrate (2 mmol; 1.5 equivalents). The solution was stirred at 70° C. for 16 hours. The reaction mixture was allowed to cool to room temperature. A white solid precipitated out. It was removed by filtration and was washed with ethanol to afford the title compound (300 mg; 87% yield). 1H NMR (400 MHz, DMSO-d6) 5.95-6.00 (2H, s), 7.00-7.05 (2H, s), 7.55-7.65 (4H, m), 9.15-9.20 (1H, s); MS (ES+) m/e=255

後処理

  1. temperatureto cool to room temperature
  2. customA white solid precipitated out
  3. customIt was removed by filtration
  4. washwas washed with ethanol

出典と根拠

ORDレコード
ord-941036632d3c47bc8da6ab45b8f950d8
出典データセット
uspto-grants-2007_10
特許番号
US07279469B2

反応ノート

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