
基本信息:
- 专利标题: 二氢黄樟素的制备方法
- 专利标题(英):Preparation method for dihydrosafrole
- 申请号:CN201110024281.0 申请日:2011-01-22
- 公开(公告)号:CN102070596A 公开(公告)日:2011-05-25
- 发明人: 陈新志 , 王帅 , 钱超
- 申请人: 浙江大学
- 申请人地址: 浙江省杭州市西湖区浙大路38号
- 专利权人: 浙江大学
- 当前专利权人: 浙江大学
- 当前专利权人地址: 浙江省杭州市西湖区浙大路38号
- 代理机构: 杭州中成专利事务所有限公司
- 代理人: 金祺
- 主分类号: C07D317/50
- IPC分类号: C07D317/50
The invention discloses a preparation method for dihydrosafrole. Piperidine and propionyl chloride are used as initial raw materials, and the preparation method comprises the following steps of: 1) acylation reaction of Friedel-crafts of the piperidine: reacting the piperidine and the propionyl chloride in a solvent I under the catalytic action of a lewis acid catalyst, adding iced water after finishing the reaction, standing, separating phases, washing an organic phase in the lower layer and distilling the solvent I to obtain piperonyl ethyl ketone; and 2) reduction reaction of Wolff-Kishner-Huang-min-lon of the piperonyl ethyl ketone: refluxing the piperonyl ethyl ketone and hydrazine hydrate solution at the mass concentration of 80 to 90 percent in a solvent II for hydrazone reaction, and adding polyethyleneglycol-400 and potassium hydroxide and performing hydrazone decomposing reaction to obtain the dihydrosafrole. The method for preparing the dihydrosafrole has the characteristics of high product yield rate, mild process condition, simple operation and the like.
公开/授权文献:
- CN102070596B 二氢黄樟素的制备方法 公开/授权日:2013-02-27
IPC结构图谱:
C | 化学;冶金 |
--C07 | 有机化学 |
----C07D | 杂环化合物 |
------C07D317/00 | 杂环化合物,含五元环,有两个氧原子作为仅有的杂环原子 |
--------C07D317/02 | .在位置1和2有杂原子 |
----------C07D317/10 | ..不和其他环稠合 |
------------C07D317/46 | ...与1个六元环稠合 |
--------------C07D317/48 | ....亚甲二氧基苯或氢化亚甲二氧基苯,杂环未取代的 |
----------------C07D317/50 | .....仅有氢原子、烃基或取代烃基,直接连在环碳原子上 |