Hydrazine hydrate (1:1) → 5-(2-fluoro-4-methoxyphenyl)-1H-pyrazol-3-amine

HRID 1507466노트

반응식

HRID 1507466 반응식
[F:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10](=O)[CH2:11][C:12]#[N:13].O.[NH2:16][NH2:17]>C(O)C>[F:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10]1[NH:17][N:16]=[C:12]([NH2:13])[CH:11]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 534039523-(2-Fluoro-4-methoxyphenyl)-3-oxopropanenitrile

생성물 1

HCID 534182315-(2-fluoro-4-methoxyphenyl)-1H-pyrazol-3-amine수율 88.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 3-(2-Fluoro-4-methoxyphenyl)-3-oxopropanenitrile (9.55 g, 49.4 mmol) suspended in ethanol (165 mL) was added hydrazine hydrate (1.743 g, 54.38 mmol). The resulting mixture was heated at reflux overnight. Then, the organic solvent was evaporated in vacuo and the resulting residue was chromatographed (eluting with 9:1 methylene chloride:methanol) to give 9.07 g (88% yield) of the title compound. LCMS (ESI): calc.=207; obs. M+H=208.2.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. customThen, the organic solvent was evaporated in vacuo
  4. customthe resulting residue was chromatographed
  5. wash(eluting with 9:1 methylene chloride:methanol)

출처 및 근거

ORD 기록
ord-5bee5a0291ef4ecab614cbe5b668ce95
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221814B2

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