
基本信息:
- 专利标题: 一种乌拉地尔药物中间体1,3-二甲基-6-(3-羟基丙基)氨基尿嘧啶的合成方法
- 专利标题(英):Synthesis method of urapidil pharmaceutical intermediate 1,3-dimethyl-6-(3-hydroxpropyl)aminouracil
- 申请号:CN201610827838.7 申请日:2016-09-18
- 公开(公告)号:CN106432101A 公开(公告)日:2017-02-22
- 发明人: 彭飞
- 申请人: 厦门市凯尔利信息科技有限公司
- 申请人地址: 福建省厦门市思明区长青路472号-302
- 专利权人: 厦门市凯尔利信息科技有限公司
- 当前专利权人: 厦门市凯尔利信息科技有限公司
- 当前专利权人地址: 福建省厦门市思明区长青路472号-302
- 优先权: 201510999312.2 2015.12.25 CN
- 主分类号: C07D239/54
- IPC分类号: C07D239/54
The invention provides a synthesis method of a urapidil pharmaceutical intermediate 1,3-dimethyl-6-(3-hydroxpropyl)aminouracil. The synthesis method comprises the following steps: adding 0.61mol of 1,3-dimethyl-6-hydroxluracil (2), 0.72mol to 0.75mol of 3-amino-1-propanol and 0.16mol of a sodium sulfite solution into a reaction container provided with a stirrer, a thermograph and a reflux condenser; controlling a stirring speed to be 130rpm to 160rpm; raising the temprature of a solution to be 150 DEG C to 160 DEG C and reacting for 90min to 120min; lowering the temprature of the solution to be 60 DEG C to 65 DEG C and adding 230ml of cyclohexane; refluxing for 30min to 50min and filtering; lowering the temperature of filtrate to be 5 DEG C to 9 DEG C; standing for 30h to 35h; separating out a crystal and filtering; washing the obtained crystal with a salt solution and then washing with acetonitrile; dehydrating the crystal with a dehydrating agent; recrystallizing in isopropyl alcohol to obtain a white crystal, namely the 1,3-dimethyl-6-(3-hydroxpropyl)aminouracil.
IPC结构图谱:
C | 化学;冶金 |
--C07 | 有机化学 |
----C07D | 杂环化合物 |
------C07D239/00 | 杂环化合物,含1,3-二嗪环或氢化1,3-二嗪环 |
--------C07D239/02 | .不与其他环稠合 |
----------C07D239/06 | ..环原子间或环原子与非环原子间有1个双键 |
------------C07D239/28 | ...有杂原子或有以3个键连杂原子、其中最多以1个键连卤素的碳原子,直接连在环碳原子上 |
--------------C07D239/32 | ....1个氧、硫或氮原子 |
----------------C07D239/52 | .....两个氧原子 |
------------------C07D239/54 | ......以双键连接的氧原子或未被取代的羟基 |