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    • 51. 发明授权
    • Preparation of 1-methylpiperazine and 1,4-dimethylpiperazine as
co-products
    • 制备1-甲基哌嗪和1,4-二甲基哌嗪作为副产物
    • US3948900A
    • 1976-04-06
    • US498188
    • 1974-08-16
    • Philip Hotchkiss Moss
    • Philip Hotchkiss Moss
    • C07D295/023C07D295/04
    • C07D295/023
    • A process for the preparation of 1-methylpiperazine and 1,4-dimethylpiperazine as co-products is disclosed which provides a crude reaction product free of piperazine impurity. The process of the invention comprises mixing and reacting formaldehyde and piperazine at a molar ratio of more than 1.3 to less than about 2.0 and then hydrogenating the resulting reaction product carried in methanol as a major solvent in liquid phase at a temperature of about 60.degree.-130.degree.C. in the presence of a nickel or cobalt hydrogenation catalyst. The crude hydrogenated reaction product is free from piperazine impurity from which 1-methylpiperazine and 1,4-dimethylpiperazine can be readily separated in substantially pure form such as by simple fractional distillation.
    • 公开了制备作为副产物的1-甲基哌嗪和1,4-二甲基哌嗪的方法,其提供了不含哌嗪杂质的粗制反应产物。 本发明的方法包括以大于1.3至小于约2.0的摩尔比混合和反应甲醛和哌嗪,然后在约60℃的温度下将所得甲醇作为主要溶剂的反应产物在液相中氢化, 130℃,在镍或钴氢化催化剂存在下。 粗制氢化反应产物不含哌嗪杂质,其中1-甲基哌嗪和1,4-二甲基哌嗪可以容易地以基本上纯的形式分离,例如通过简单的分馏。