HCID 178514519、化合物 → 2-(2,6-dichloro-4-fluorophenyl)-7-fluoro-2H-pyrazolo[4,3-c]pyridine

HRID 626742ノート

反応式

HRID 626742 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:18]([Cl:19])=[CH:17][C:16]([F:20])=[CH:15][C:14]=1[Cl:21])=[N+]=[N-]>C1(C)C=CC=CC=1>[Cl:21][C:14]1[CH:15]=[C:16]([F:20])[CH:17]=[C:18]([Cl:19])[C:13]=1[N:12]1[CH:11]=[C:5]2[CH:6]=[N:7][CH:8]=[C:9]([F:10])[C:4]2=[N:1]1

参加物

3

反応物 1

HCID 178514519HCID 178514519、化合物

生成物 1

HCID 696717192-(2,6-dichloro-4-fluorophenyl)-7-fluoro-2H-pyrazolo[4,3-c]pyridine収率 77%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of [1-(4-azido-5-fluoropyridin-3-yl)-meth-(E)-ylidene]-(2,6-dichloro-4-fluorophenyl)-amine (14.7 mmol) in toluene (40 mL) was heated under reflux for 16 hours then allowed to cool to room temperature. The reaction mixture was concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (0-50% ethyl acetate in cyclohexane) to afford the title compound as an off-white solid (3.38 g, 77% yield). LCMS (Method D): RT=2.84 min, m/z: 300 [M+H+].

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customThe residue was purified by silica gel flash chromatography (0-50% ethyl acetate in cyclohexane)

出典と根拠

ORDレコード
ord-acec05edc0a04d8fb28f51abed48e466
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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