Hydrazine hydrate (1:1) → HCID 178507275, 화합물

HRID 1452762노트

반응식

HRID 1452762 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178507275HCID 178507275, 화합물수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-cf2a90acd4ae4546a4e7a39e4b0f4390
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07473783B2

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