Bromine → 3-Bromo-5-(pyrazin-2-yl)pyridin-2(1H)-one

HRID 1981515ノート

反応式

HRID 1981515 の反応式
[Br:1]Br.[N:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[CH:11][C:12](=[O:15])[NH:13][CH:14]=1>C(O)(=O)C>[Br:1][C:11]1[C:12](=[O:15])[NH:13][CH:14]=[C:9]([C:4]2[CH:5]=[N:6][CH:7]=[CH:8][N:3]=2)[CH:10]=1

参加物

4

反応物 2

HCID 24408BromineHCID 233188115-(Pyrazin-2-yl)pyridin-2(1H)-one

生成物 1

HCID 136451023-Bromo-5-(pyrazin-2-yl)pyridin-2(1H)-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
50 °C

実験手順

3 ml of bromine are added to a stirred suspension of 5-(2-pyrazinyl)-2(1H)-pyridone (9.0 g) in 300 ml of glacial acetic acid warmed to a temperature of 50° C. The mixture is stirred at RT overnight, cooled in an ice bath to 16° C. and filtered. The filtered yellow solid is suspended in 100 ml of distilled H2O, to which sodium bisulfite is gradually added until the solid appears tan. A saturated potassium carbonate solution is slowly added until the pH is adjusted to 7.4, and the suspension is filtered. The filtered solid is washed with H2O and dried under high vacuum at 100° C. for 4 hours, giving the desired 3-bromo-5-(2-pyrazinyl)-2(1H)-pyridone which is recrystallized from methanol, M.P.>250° C.

後処理

  1. temperaturecooled in an ice bath to 16° C.
  2. filtrationfiltered
  3. additionis gradually added until the solid
  4. additionA saturated potassium carbonate solution is slowly added until the pH
  5. filtrationthe suspension is filtered
  6. washThe filtered solid is washed with H2O
  7. customdried under high vacuum at 100° C. for 4 hours

出典と根拠

ORDレコード
ord-8dfbce78f8d5433cbf835a4a6abf43c4
出典データセット
uspto-grants-1986_06
特許番号
US04593028

反応ノート

読み込み中…