2-chloro-benzoic acid N'-(5-bromo-pyridin-2-yl)hydrazide → 6-Bromo-3-(2-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyridine

HRID 2252318ノート

反応式

HRID 2252318 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH:9][C:10](=O)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[N:6][CH:7]=1>O=P(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])=[N:9][N:8]=2)[CH:7]=1

参加物

3

反応物 1

HCID 692020042-chloro-benzoic acid N'-(5-bromo-pyridin-2-yl)hydrazide

生成物 1

HCID 179744786-Bromo-3-(2-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyridine収率 30.3%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

反応条件

温度
85 °C

実験手順

A mixture of 2-chloro-benzoic acid N′-(5-bromo-pyridin-2-yl)hydrazide (2.96 g, 9.1 mmol) in POCl3 (15 mL) was heated at 85° C. for 48 hours. The solvent was removed in vacuo, and the residue quenched with saturated Na2CO3 and EtOAc. The layers were separated, and the organic layer concentrated in vacuo to minimal volume. The resulting solid was filtered and purified by flash chromatography to give the title compound (0.85 g, 30%).

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residue quenched with saturated Na2CO3 and EtOAc
  3. customThe layers were separated
  4. concentrationthe organic layer concentrated in vacuo to minimal volume
  5. filtrationThe resulting solid was filtered
  6. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-e69de3ba1c004d21b1ba54520bbbb072
出典データセット
uspto-grants-2008_01
特許番号
US07321040B2

反応ノート

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