Methyl iodide → 2-Methyl-2H-indazole-7-carbonitrile

HRID 2167683ノート

反応式

HRID 2167683 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[C:10]#[N:11])[CH:3]=[N:2]1.[C:12]([O-])([O-])=O.[Cs+].[Cs+].CI>C(#N)C>[CH3:12][N:2]1[CH:3]=[C:4]2[C:9]([C:8]([C:10]#[N:11])=[CH:7][CH:6]=[CH:5]2)=[N:1]1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 250226851H-Indazole-7-carbonitrile

生成物 1

HCID 441192602-Methyl-2H-indazole-7-carbonitrile

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 1H-indazole-7-carbonitrile (1 equiv.) in acetonitrile, Cs2CO3 (1.3 equiv.) and MeI (3 equiv.) was added and reaction was heated at 80 oC for 1.5 h. On completion, it was cooled and quenched by addition of water. Extraction was carried out using ethyl acetate. Organic layer was dried over Na2SO4 and crude compound was column purified to afford the title compound. (Polar isomer confirmed as N-2-Methyl and non-polar isomer confirmed as N-1-Methyl by NOE experimentation).

後処理

  1. customreaction
  2. temperaturewas heated at 80 oC for 1.5 h
  3. temperatureOn completion, it was cooled
  4. customquenched by addition of water
  5. extractionExtraction
  6. dry with materialOrganic layer was dried over Na2SO4 and crude compound
  7. custompurified

出典と根拠

ORDレコード
ord-1b9d0df2249c4119be46a854613f7786
出典データセット
uspto-grants-2015_06
特許番号
US09045477B2

反応ノート

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