3-Chloro-2,5-dimethylpyrazine → 2,5-Dimethyl-3-[4-(phenylmethyl)piperazin-1-yl]pyrazine

HRID 1727180ノート

反応式

HRID 1727180 の反応式
Cl[C:2]1[C:3]([CH3:9])=[N:4][CH:5]=[C:6]([CH3:8])[N:7]=1.[CH2:10]([N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])O.[Na+]>>[CH3:9][C:3]1[C:2]([N:20]2[CH2:21][CH2:22][N:17]([CH2:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:18][CH2:19]2)=[N:7][C:6]([CH3:8])=[CH:5][N:4]=1

参加物

4

反応物 3

HCID 667713-Chloro-2,5-dimethylpyrazineHCID 759941-BenzylpiperazineHCID 516892Sodium Bicarbonate

生成物 1

HCID 690591832,5-Dimethyl-3-[4-(phenylmethyl)piperazin-1-yl]pyrazine収率 58%

反応条件

温度
125 °C

実験手順

3-Chloro-2,5-dimethylpyrazine (1.0 g, 7.0 mmol) and N-benzylpiperazine (3.7 ml, 21.0 mmol) were mixed under nitrogen and heated to 125° C. for 18 h. Saturated aqueous sodium hydrogen carbonate was added and the product was extracted with chloroform. The combined organic extracts were dried (Na2SO4) and concentrated in vacuo to give a yellow oil. The crude product was purified by flash chromatography using silica gel eluting with methanol:chloroform (2.5:97.5) to give the pure product as a yellow oil (1.14 g, 58%).

後処理

  1. extractionthe product was extracted with chloroform
  2. dry with materialThe combined organic extracts were dried (Na2SO4)
  3. concentrationconcentrated in vacuo
  4. customto give a yellow oil
  5. customThe crude product was purified by flash chromatography

出典と根拠

ORDレコード
ord-145e06f18d0d4bf9b74108aadfdb0624
出典データセット
uspto-grants-2009_02
特許番号
US07494992B2

反応ノート

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