HCID 178510122、化合物 → 3-Chloro-5-fluoro-2-(7-fluoropyrazolo[4,3-c]pyridin-2-yl)-benzonitrile

HRID 626782ノート

反応式

HRID 626782 の反応式
[N:1]([C:4]1[C:9]([F:10])=[CH:8][N:7]=[CH:6][C:5]=1/[CH:11]=[N:12]/[C:13]1[C:20]([Cl:21])=[CH:19][C:18]([F:22])=[CH:17][C:14]=1[C:15]#[N:16])=[N+]=[N-]>C1(C)C=CC=CC=1>[Cl:21][C:20]1[C:13]([N:12]2[CH:11]=[C:5]3[CH:6]=[N:7][CH:8]=[C:9]([F:10])[C:4]3=[N:1]2)=[C:14]([CH:17]=[C:18]([F:22])[CH:19]=1)[C:15]#[N:16]

参加物

3

反応物 1

HCID 178510122HCID 178510122、化合物

生成物 1

HCID 696715683-Chloro-5-fluoro-2-(7-fluoropyrazolo[4,3-c]pyridin-2-yl)-benzonitrile収率 93%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 2-{[1-(4-azido-5-fluoropyridin-3-yl)-meth-(E)-ylidene]-amino}-3-chloro-5-fluorobenzonitrile (1.67 g, 5.25 mmol) in anhydrous toluene (25 mL) was heated under reflux for 4.5 hours. The resultant mixture was allowed to cool to room temperature and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (0-5% methanol in DCM) to afford the title compound as a yellow solid (1.41 g, 93% yield). LCMS (Method C): RT=2.71 min, m/z: 291 [M+H+].

後処理

  1. temperatureunder reflux for 4.5 hours
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was purified by silica gel flash chromatography (0-5% methanol in DCM)

出典と根拠

ORDレコード
ord-514e778e05a64fccaa7634d7029e9b2d
出典データセット
uspto-grants-2016_04
特許番号
US09309240B2

反応ノート

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