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

HRID 493319노트

반응식

HRID 493319 반응식
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

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 785752,3-Dichloropyrazine

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-82c2c44ed4c64d36b80d7c03f72a40a5
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534794B2

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