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

HRID 1049158노트

반응식

HRID 1049158 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
75 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-28efc1b79d6e4df29d9be3845dd7db0d
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382237B2

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