N-甲基哌嗪 → 2-氯-3-(4-甲基哌嗪-1-基)吡嗪

HRID 991663笔记

反应方程式

HRID 991663 反应方程式
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

参与物

4

反应物 2

HCID 53167N-甲基哌嗪HCID 785752,3-二氯吡嗪

产物 1

HCID 220363522-氯-3-(4-甲基哌嗪-1-基)吡嗪收率 75%

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-f543c41e355f43cd9a16c7631bbd89cc
来源数据集
uspto-grants-2002_10
专利号
US06465467B1

反应笔记

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