1-Methylpiperazine → 2-Chloro-3-(4-methylpiperazin-1-YL)pyrazine

HRID 493319ノート

反応式

HRID 493319 の反応式
Cl[C:2]1[C:7]([Cl:8])=[N:6][CH:5]=[CH:4][N:3]=1.[CH3:9][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C(#N)C>[Cl:8][C:7]1[C:2]([N:13]2[CH2:14][CH2:15][N:10]([CH3:9])[CH2:11][CH2:12]2)=[N:3][CH:4]=[CH:5][N:6]=1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 785752,3-Dichloropyrazine

生成物 1

HCID 220363522-Chloro-3-(4-methylpiperazin-1-YL)pyrazine収率 75%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 2,3-dichloropyrazine (10.1 g, 68 mmol) and N-methylpiperazine (10.15 g, 100 mmol) in acetonitrile (250 mL) was stirred at room temperature for 60 h. The solvent was removed under reduced pressure and the residue was taken up in CHCl3/brine. The dried (MgSO4) organic layer was concentrated and the remaining oil was purified by chromatography on silica gel using CHCl3/MeOH (95:5) as eluent to give 10.7 g (75%) of the title compound as an oil that crystallized upon standing: mp 34-36° C. Anal. (C9H13ClN4) C, H, N.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dry with materialThe dried (MgSO4) organic layer
  3. concentrationwas concentrated
  4. customthe remaining oil was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-82c2c44ed4c64d36b80d7c03f72a40a5
出典データセット
uspto-grants-2009_05
特許番号
US07534794B2

反応ノート

読み込み中…