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

HRID 991663노트

반응식

HRID 991663 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-f543c41e355f43cd9a16c7631bbd89cc
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06465467B1

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