Hydrazine hydrate (1:1) → HCID 178507275、化合物

HRID 1452762ノート

反応式

HRID 1452762 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=O)[CH2:9][C:10]#[N:11].O.[NH2:14][NH2:15]>CCO>[NH2:11][C:10]1[NH:15][N:14]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Br:1])[CH:9]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 107043343-(2-Bromophenyl)-3-oxopropanenitrile

生成物 1

HCID 178507275HCID 178507275、化合物収率 70%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 3-(2-bromo-phenyl)-3-oxo-propionitrile (1.8 g, 8.03 mmol) in absolute EtOH (25 mL) was added hydrazine hydrate (2.3 mL, 48.2 mmol). The reaction mixture was refluxed for 23 hours, then cooled and purified directly on silica gel with 0-10% MeOH in CH2Cl2 as eluent to provide 1.33 g (70% yield) of 5-amino-3-(2-bromophenyl)pyrazole as a sticky oil. 1H-NMR (d6-DMSO) δ: 11.7 (broad m, 1H, tautomers), 7.20-7.70 (broad m, 4H), 5.76 (broad m, 1H), 5.03 (broad s, 1H), 4.60 (broad s, 1H); HPLC/MS m/z: 238.0, 240.0 [MH]+.

後処理

  1. temperatureThe reaction mixture was refluxed for 23 hours
  2. temperaturecooled
  3. custompurified directly on silica gel with 0-10% MeOH in CH2Cl2 as eluent

出典と根拠

ORDレコード
ord-cf2a90acd4ae4546a4e7a39e4b0f4390
出典データセット
uspto-grants-2009_01
特許番号
US07473783B2

反応ノート

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