Pyridine-2-carbonitrile → HCID 59750419、化合物

HRID 748095ノート

反応式

HRID 748095 の反応式
[F:1][C:2]1[C:7]([C:8]([OH:10])=O)=[C:6]([SH:11])[CH:5]=[CH:4][CH:3]=1.[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1)#[N:13]>N1C=CC=CC=1>[F:1][C:2]1[C:7]2[C:8](=[O:10])[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[S:11][C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 7522Pyridine-2-carbonitrileHCID 229394662-Fluoro-6-sulfanylbenzoic acid

生成物 1

HCID 59750419HCID 59750419、化合物収率 1.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
135 °C

実験手順

A mixture of 6-fluoro-2-mercaptobenzoic acid (5.00 g, 29.0 mmol), 2-cyanopyridine (3.05 g, 29.3 mmol) and pyridine (30.0 ml) was refluxed at 135° C. for 48 hrs as described in Example 9. The reaction mixture was concentrated. The residue was subjected to a silica gel column chromatography and eluted with hexane-ethyl acetate (2:1, v/v). The resultant product was recrystallized from ethanol to give the titled compound (0.11 g, 1%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. washeluted with hexane-ethyl acetate (2:1
  3. customThe resultant product was recrystallized from ethanol

出典と根拠

ORDレコード
ord-66df7830dc9c461ea6c2de727230d18a
出典データセット
uspto-grants-2008_07
特許番号
US07399759B2

反応ノート

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