Hydrazine hydrate (1:1) → 5-amino-3-((4-(dimethylamino)phenyl)amino)-1H-pyrazole-4-carboxamide

HRID 1049158ノート

反応式

HRID 1049158 の反応式
[C:1]([C:3](=[C:7]([NH:10][C:11]1[CH:16]=[CH:15][C:14]([N:17]([CH3:19])[CH3:18])=[CH:13][CH:12]=1)SC)[C:4]([NH2:6])=[O:5])#[N:2].O.[NH2:21][NH2:22]>C(O)C>[NH2:2][C:1]1[NH:22][N:21]=[C:7]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([N:17]([CH3:19])[CH3:18])=[CH:13][CH:12]=2)[C:3]=1[C:4]([NH2:6])=[O:5]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 867018642-Cyano-3-((4-(dimethylamino)phenyl)amino)-3-(methylthio)acrylamide

生成物 1

HCID 867018655-amino-3-((4-(dimethylamino)phenyl)amino)-1H-pyrazole-4-carboxamide収率 72%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
75 °C

実験手順

2-cyano-3-((4-(dimethylamino)phenyl)amino)-3-(methylthio)acrylamide (0.997 g) was suspended in 10 mL of ethanol and hydrazine hydrate (337 μL, 1.5 eq.) was added drop wise to the reaction. The reaction was then heated at 75° C. until the starting material was no longer present and confirmed via HPLC. Once starting material was absent (18 hrs), reaction was brought to room temperature and filtered to obtain 5-amino-3-((4-(dimethylamino)phenyl)amino)-1H-pyrazole-4-carboxamide as an off white to yellow powder. The product was allowed to dry under vacuum for 1 hr (900 mg, 72% yield).

後処理

  1. customwise to the reaction
  2. custom(18 hrs), reaction
  3. customwas brought to room temperature
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-28efc1b79d6e4df29d9be3845dd7db0d
出典データセット
uspto-grants-2016_07
特許番号
US09382237B2

反応ノート

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