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    • 36. 发明授权
    • Preparation of 3-methylpiperidine
    • 3-甲基哌啶的制备
    • US3975392A
    • 1976-08-17
    • US591184
    • 1975-06-27
    • Lawson G. Wideman
    • Lawson G. Wideman
    • C07D295/02C07D295/027
    • C07D295/027
    • There is disclosed a process for the preparation of 3-methylpiperidine which comprises a multi-stage hydrogenation of .alpha.-methylene glutaronitrile using as a catalyst a highly dispersed nickel in which the first stage hydrogenation is conducted at temperature ranging from about 20.degree.C to about 50.degree.C at hydrogen pressure of at least 14 kilograms per square centimeter to form .alpha.-methyl glutaronitrile. The second stage hydrogenation is conducted at temperatures ranging from about 80.degree.C to about 175.degree.C at hydrogen pressures of at least 42 kilograms per square centimeter to form 2-methyl-1,5-diaminopentane. At which time the reaction mixture is cooled to a temperature below the boiling point of any of the materials present in the process and all the excess hydrogen vented off. The temperature is then increased to at least about 150.degree.C to allow the 2-methyl-1,5-diaminopentane to cyclize to form 3-methylpiperidine.
    • 公开了一种制备3-甲基哌啶的方法,其包括使用高度分散的镍作为催化剂的α-亚甲基戊二腈的多级氢化,其中第一阶段氢化在约20℃至约20℃的温度范围内进行 50℃,氢压至少14千克/平方厘米,形成α-甲基戊二腈。 第二阶段氢化在约80℃至约175℃的温度下进行,氢压至少为42千克每平方厘米,形成2-甲基-1,5-二氨基戊烷。 此时将反应混合物冷却到低于该方法中存在的任何物质的沸点的温度,并且所有过量的氢气排出。 然后将温度升至至少约150℃,以使2-甲基-1,5-二氨基戊烷环化形成3-甲基哌啶。