Chlorine → 3-Chloro-5-(trifluoromethyl)pyridin-2-ol

HRID 464127

反応式

HRID 464127 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[CH:5][C:6](=[O:9])[NH:7][CH:8]=1.[Cl:12]Cl>C(Cl)(Cl)Cl>[Cl:12][C:5]1[C:6](=[O:9])[NH:7][CH:8]=[C:3]([C:2]([F:1])([F:10])[F:11])[CH:4]=1

参加物

4

反応物 2

HCID 24526ChlorineHCID 1474432-Hydroxy-5-(trifluoromethyl)pyridine

生成物 1

HCID 7254363-Chloro-5-(trifluoromethyl)pyridin-2-ol

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

[A] 0.2 g of 5-trifluoromethyl-2-pyridone was dissolved in 20 ml of chloroform, and chlorine gas was pressed through the solution at 50° C. for 1 hour while stirring. After completion of the reaction, the chloroform was distilled off, and recrystallization was performed from a mixed solvent of toluene and n-hexane to obtain 0.15 g of the titled compound having a melting point of 144° to 147° C. The recrystallization was further repeated to obtain 0.09 g of the titled compound having a melting point of 165° to 166° C.

後処理

  1. customAfter completion of the reaction
  2. distillationthe chloroform was distilled off
  3. customrecrystallization

出典と根拠

ORDレコード
ord-3d65025180d541d09500a4a4ae4da374
出典データセット
uspto-grants-1985_10
特許番号
US04546191

関連ノート

読み込み中…