Hydrazine hydrate (1:1) → 3-(1,3-benzodioxol-5-yl)-N-[4-(hydrazinocarbonyl)phenyl]propanamide

HRID 642169

反応式

HRID 642169 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][C:12]([NH:14][C:15]3[CH:24]=[CH:23][C:18]([C:19](OC)=[O:20])=[CH:17][CH:16]=3)=[O:13])=[CH:9][C:4]=2[O:3][CH2:2]1.O.[NH2:26][NH2:27]>CCO>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][C:12]([NH:14][C:15]3[CH:24]=[CH:23][C:18]([C:19]([NH:26][NH2:27])=[O:20])=[CH:17][CH:16]=3)=[O:13])=[CH:9][C:4]=2[O:3][CH2:2]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 9945244Methyl 4-{[3-(1,3-benzodioxol-5-yl)propanoyl]amino}benzoate

生成物 1

HCID 98585743-(1,3-benzodioxol-5-yl)-N-[4-(hydrazinocarbonyl)phenyl]propanamide収率 65%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of methyl 4-{[3-(1,3-benzodioxol-5-yl)propanoyl]amino}benzoate (200 mg, 0.61 mmol) in EtOH (3.5 mL) was added hydrazine hydrate (0.5 mL). After stirring for 15 hrs at reflux, the reaction mixture was cooled to rt and a white solid precipitated out. Filtration, washing with EtOH (2×1 mL) and water (3×1 mL), and drying under vacuo at 70° C. for 1 hr gave 130 mg of the title compound (65%) as a white solid in 95.5% 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 (2×1 mL) and water (3×1 mL)
  5. customdrying under vacuo at 70° C. for 1 hr

出典と根拠

ORDレコード
ord-a7e4da2c8d7c43bb97c5b0b8310c96f7
出典データセット
uspto-grants-2010_04
特許番号
US07696231B2

関連ノート

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