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

HRID 1507466ノート

反応式

HRID 1507466 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-5bee5a0291ef4ecab614cbe5b668ce95
出典データセット
uspto-grants-2015_12
特許番号
US09221814B2

反応ノート

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