Chlorine → 3-Chloro-1-methyl-5-(pyrazin-2-yl)pyridin-2(1H)-one

HRID 1388662ノート

反応式

HRID 1388662 の反応式
[Cl:1]Cl.[CH3:3][N:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[N:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:6][C:5]1=[O:16]>C(O)(=O)C>[Cl:1][C:6]1[C:5](=[O:16])[N:4]([CH3:3])[CH:9]=[C:8]([C:10]2[CH:15]=[N:14][CH:13]=[CH:12][N:11]=2)[CH:7]=1

参加物

4

反応物 2

HCID 24526Chlorine2 回HCID 136450981-Methyl-5-(pyrazin-2-yl)pyridin-2(1H)-one

生成物 1

HCID 136451003-Chloro-1-methyl-5-(pyrazin-2-yl)pyridin-2(1H)-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

About 1.2 ml of condensed chlorine gas is introduced into a reaction mixture comprising 1-methyl-5-(2-pyrazinyl)-2-pyridone (3.2 g) dissolved in 200 ml of glacial acetic acid. After all the chlorine is added, stirring is stopped and the solid product filtered, washed with ether and air dried. The dried solid is suspended in distilled H2O to which saturated potassium carbonate is added until the pH is greater than 7. The resulting white solid is filtered, recrystallized from isopropanol, and NMR and IR indicate that it is the desired 3-chloro-1-methyl-5-(2-pyrazinyl)-2-pyridone compound, M.P. 197°-198° C.

後処理

  1. filtrationthe solid product filtered
  2. washwashed with ether and air
  3. customdried
  4. additionis added until the pH is greater than 7
  5. filtrationThe resulting white solid is filtered
  6. customrecrystallized from isopropanol, and NMR and IR

出典と根拠

ORDレコード
ord-51e4b8488b3445e4949a0f62864d4886
出典データセット
uspto-grants-1984_02
特許番号
US04432979

反応ノート

読み込み中…