Sodium hydride → 2-Bromo-5-(4-methylpiperazin-1-YL)pyrazine

HRID 1157808ノート

反応式

HRID 1157808 の反応式
[H-].[Na+].[CH3:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.Br[C:11]1[C:16]([Br:17])=[N:15][CH:14]=[CH:13][N:12]=1>C1COCC1>[Br:17][C:16]1[CH:11]=[N:12][C:13]([N:7]2[CH2:8][CH2:9][N:4]([CH3:3])[CH2:5][CH2:6]2)=[CH:14][N:15]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 531671-MethylpiperazineHCID 138675722,3-Dibromopyrazine

生成物 1

HCID 457877252-Bromo-5-(4-methylpiperazin-1-YL)pyrazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To sodium hydride (0.20 g) taken in dry THF (15 ml), N-methyl piperazine (0.93 ml) was added under nitrogen at 0° C. 2,3-Dibromopyrazine (2 g) taken in 15 ml dry THF was added to the above mixture at 0° C. The reaction mixture was allowed to reflux for overnight and quenched with water (5 ml). The organic layer was removed under vacuum. The resulting crude mass was purified by column chromatography to afford 2-bromo-5-(4-methylpiperazin-1-yl)pyrazine as pure product.

後処理

  1. additionwas added to the above mixture at 0° C
  2. temperatureto reflux for overnight
  3. customquenched with water (5 ml)
  4. customThe organic layer was removed under vacuum
  5. customThe resulting crude mass was purified by column chromatography

出典と根拠

ORDレコード
ord-ba9d85b3054f4180892a28bc5e1e1f26
出典データセット
uspto-grants-2010_10
特許番号
US07807676B2

反応ノート

読み込み中…