CN110642775A - 一种二甲基哌啶的合成方法 - Google Patents
一种二甲基哌啶的合成方法 Download PDFInfo
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- CN110642775A CN110642775A CN201810676458.7A CN201810676458A CN110642775A CN 110642775 A CN110642775 A CN 110642775A CN 201810676458 A CN201810676458 A CN 201810676458A CN 110642775 A CN110642775 A CN 110642775A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D211/00—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings
- C07D211/04—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D211/06—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D211/08—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hydrocarbon or substituted hydrocarbon radicals directly attached to ring carbon atoms
- C07D211/10—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hydrocarbon or substituted hydrocarbon radicals directly attached to ring carbon atoms with radicals containing only carbon and hydrogen atoms attached to ring carbon atoms
- C07D211/12—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hydrocarbon or substituted hydrocarbon radicals directly attached to ring carbon atoms with radicals containing only carbon and hydrogen atoms attached to ring carbon atoms with only hydrogen atoms attached to the ring nitrogen atom
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- Organic Chemistry (AREA)
- Hydrogenated Pyridines (AREA)
Abstract
本发明公开了一种二甲基哌啶的合成方法，将3,5‑二甲基吡啶加入高压釜，加入有机溶剂和定量催化剂，升温到90~160℃，加压到3MPa~10MPa，通入氢气还原即可得；本发明工艺简单实用，操作方便，收率高，无毒无害，适合企业化生产。
Description
技术领域
本发明属于化合物合成技术领域，具体是一种二甲基哌啶的合成方法。
背景技术
3,5-二甲基哌啶是合成大环内酯类新型抗菌素替米考星的重要原料，作为药物中间体，3,5-二甲基哌啶主要要求顺式结构占85%，反式结构占15%。通过3,5-二甲基吡啶加氢还原的方法是大量获取3,5-二甲基哌啶的最佳途径。
发明内容
本发明的目的就是提供一种工艺简单实用，操作方便，收率高的二甲基吡啶合成方法。
本发明是通过以下技术方案实现的：将3,5-二甲基吡啶加入高压釜，加入有机溶剂和定量催化剂，升温到90~160℃，加压到3MPa~10MPa，通入氢气还原即可得
本发明中有机溶剂为甲醇、乙醇或四氢呋喃中的任意一种。
本发明有益效果为：工艺简单实用，操作方便，收率高，无毒无害，适合企业化生产，大大降低了企业生产成本，且摩尔收率高达85%以上。
具体实施方式
实施例1
在200ml高压釜中，投入100ml甲醇，加入10ml 3,5-二甲基吡啶，加入Pd/C催化剂0.5g，升温至140℃，通氢气加压至9Mpa，直至吸氢结束，保温反应5小时，降温滤除反应液，精馏得到3,5-二甲基哌啶，气相检测，顺式结构87%。
实施例2
在200ml高压釜中，投入100ml乙醇，加入10ml 3,5-二甲基吡啶，加入Pd/C催化剂0.5g，升温至150℃，通氢气加压至9.5Mpa，直至吸氢结束，保温反应5小时，降温滤除反应液，精馏得到3,5-二甲基哌啶，气相检测，顺式结构90%。
Claims (2)
1.一种二甲基哌啶的合成方法，其特征在于：将3,5-二甲基吡啶加入高压釜，加入有机溶剂和定量催化剂，升温到90~160℃，加压到3MPa~10MPa，通入氢气还原即可得。
2.根据权利要求1所述的一种二甲基哌啶的合成方法，其特征是：所述有机溶剂为甲醇、乙醇或四氢呋喃中的任意一种。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113372262A (zh) * | 2021-06-08 | 2021-09-10 | 安徽星宇化工有限公司 | 一种反式3,5-二甲基哌啶的制备方法 |
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2018
- 2018-06-27 CN CN201810676458.7A patent/CN110642775A/zh active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113372262A (zh) * | 2021-06-08 | 2021-09-10 | 安徽星宇化工有限公司 | 一种反式3,5-二甲基哌啶的制备方法 |
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Application publication date: 20200103 |