Hydrazine hydrate (1:1) → HCID 9923619、化合物

HRID 642103ノート

反応式

HRID 642103 の反応式
[C:1]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:6]=[CH:5][C:4]([C:7]([NH:9][C:10]2[CH:19]=[CH:18][C:13]([C:14](OC)=[O:15])=[CH:12][CH:11]=2)=[O:8])=[CH:3][CH:2]=1.O.[NH2:27][NH2:28]>CCO>[NH:27]([C:14]([C:13]1[CH:18]=[CH:19][C:10]([NH:9][C:7]([C:4]2[CH:5]=[CH:6][C:1]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:2][CH:3]=2)=[O:8])=[CH:11][CH:12]=1)=[O:15])[NH2:28]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 2838376HCID 2838376、化合物

生成物 1

HCID 9923619HCID 9923619、化合物収率 66%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of methyl 4-[([1,1′-biphenyl]-4-ylcarbonyl)amino]benzoate (880 mg, 2.66 mmol) in EtOH (10 mL) was added hydrazine hydrate (1.8 mL). After stirring for 7 days at reflux, the reaction mixture was cooled to rt and a white solid precipitated out. Filtration, washing with EtOH (3×2 mL) and water (3×2 mL), and drying under vacuo at rt for 6 hrs gave 585 mg of the title compound (66%) as a white solid in 96.4% purity by HPLC (MaxPlot detection between 230 and 400 nm).

後処理

  1. temperatureat reflux
  2. customa white solid precipitated out
  3. filtrationFiltration
  4. washwashing with EtOH (3×2 mL) and water (3×2 mL)
  5. customdrying under vacuo at rt for 6 hrs

出典と根拠

ORDレコード
ord-392b98687bde47559601684becb0b56e
出典データセット
uspto-grants-2010_04
特許番号
US07696231B2

反応ノート

読み込み中…