Acetic Anhydride → HCID 136199666、化合物

HRID 263570ノート

反応式

HRID 263570 の反応式
[C:1]1([C:7]2[N:8]=[C:9]([C:12]3[CH:13]=[N+:14]([O-])[CH:15]=[CH:16][CH:17]=3)[S:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(OC(=O)C)(=[O:21])C>>[O:21]=[C:13]1[C:12]([C:9]2[S:10][CH:11]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[N:8]=2)=[CH:17][CH:16]=[CH:15][NH:14]1

参加物

3

実験手順

In 25 ml of acetic anhydride was dissolved 2.8 g of 3-(4-phenylthiazol-2-yl)pyridine-N-oxide. The solution was refluxed for 6 hours with heating. The solvent was removed by distillation. The residue was treated with ammonia water and extracted with dichloromethane. The extract was water-washed, dried and subjected to solvent removal by distillation. The residue was mixed with a small amount of dichloromethane. The resulting crystals were collected by filtration and recrystallized from methanol to obtain 60 mg of 2-(2-oxopyridin-3-yl)4-phenylthiazole as light brown plate crystals.

後処理

  1. temperatureThe solution was refluxed for 6 hours
  2. temperaturewith heating
  3. customThe solvent was removed by distillation
  4. additionThe residue was treated with ammonia water
  5. extractionextracted with dichloromethane
  6. washwashed
  7. customdried
  8. customsubjected to solvent removal by distillation
  9. additionThe residue was mixed with a small amount of dichloromethane
  10. filtrationThe resulting crystals were collected by filtration
  11. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-ca93c77a03fc4ab6a8c39369d389e9f7
出典データセット
uspto-grants-1997_07
特許番号
US05643932

反応ノート

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