CN107253906A - 一种高效环保敌鼠钠盐制备工艺方法 - Google Patents
一种高效环保敌鼠钠盐制备工艺方法 Download PDFInfo
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- C07C29/36—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal
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Abstract
本发明涉及一种高效环保敌鼠钠盐制备工艺方法，本路线从苯基格氏试剂和乳酸酯出发，首先通过格式反应生成1,1‑二苯基‑1，2‑丙二醇；然后将1,1‑二苯基‑1，2‑丙二醇在硫酸中脱水，合成出偏二苯基丙酮；偏二苯基丙酮首先和邻苯二甲酸二甲酯缩合，然后用氢氧化钠碱化，即得到敌鼠钠盐。本发明能够提供一种操作方便、工艺简化、收率高、生产成本低、三废少、环境友好且便于工业化生产的敌鼠钠盐制备工艺方法。
Description
技术领域
本发明属于有机合成化学领域，亦属于农药领域，具体涉及一种高效环保敌鼠钠盐制备工艺方法。
背景技术
敌鼠钠盐（CAS：42721-99-3）属于茚满二酮类化合物，是一种抗凝血杀鼠剂，其多次口服毒力远大于急性口服毒力，因此累计毒力效果明显，灭鼠效果好，而且有特效解毒药Vk1，因此对人畜相对安全，故得到比较广泛的推广。
敌鼠钠盐的早期的合成路线，多是从苯基丙酮出发，经过溴化或者氯化，然后再苯基化，和邻苯二甲酸二甲酯环合，酸化得到敌鼠，再把敌鼠转化成敌鼠钠盐，其工艺路线如下：
美国Upjohn公司采用苯基丙酮溴化的方法；前苏联莫斯科化工学院学报报道了以氯化亚替代液溴，通过氯化来推进反应。从上述工艺路线图可以看出，其工艺路线比较长，因此生产成本高，产量低，以上路线无论是氯化还是溴化，都会产生大量废水，对设备损害也比较大。
为克服上述缺点，又开发出一种新的工艺路线，即从丙酮出发，进过一次氯化产生一氯丙酮，然后二次氯化得到1.1.1-三氯丙酮，再还原得1.1.1-三氯异丙醇，经过苯基化产生偏二苯基丙酮，最后环化得到敌鼠钠盐，其反应工艺路线图如下：
该工艺路线原料价格低，易得，和早期得工艺相比有所改进，但路线仍然比较长；而且使用到了氯气，危险性较大，对设备要求和损害都比较高，特别是制备1.1.1-三氯丙酮得时候，副反应比较多，产品纯度低，不易纯化；大量使用异丙醇铝，三氯化铝等，废水很大，不符合环保要求。
发明内容
本发明目的是为了克服现有技术的不足而提供一种操作方便、工艺简化、收率高、生产成本低、三废少、对环境友好且便于工业化生产的敌鼠钠盐制备工艺方法。
为达到上述目的，本发明采用了如下技术方案：
一种高效环保敌鼠钠盐制备工艺方法，其合成工艺路线为：
包括以下步骤：
步骤一：苯基格氏试剂和乳酸酯反应，生成1,1-二苯基-1，2-丙二醇，即中间体1；
步骤二：将所述步骤一得到的中间体1在硫酸中脱水，合成得到偏二苯基丙酮；
步骤三：将所述步骤一得到的偏二苯基丙酮首先和邻苯二甲酸二甲酯进行缩合，然后用氢氧化钠碱化，最后得到敌鼠钠盐。
由于上述技术方案的运用，本发明具有的益技术效果：本技术方案的工艺路线短，生产步骤更加简化、效率更高、原材料简便易得、生产成本低、价格便宜；另外也避免使用对设备要求高、损害大得氯气或者液溴等原料，同时也没有使用高毒得苯试剂以及铝化物等，更安全环保。
附图说明
下面结合具体实施例对本发明作进一步的详细说明。
图1为本发明整体工艺路线示意图。
具体实施方式
下面结合附图及具体实施例对本发明作进一步的详细说明。
一、偏二苯基丙酮的制备
试验物料：
| 名 称 | 分子量 | 投料量 | 摩尔比 | 纯度 |
| 甲醇钠 | 54.02 | 21g | 1.3 | 30% |
| 邻苯二甲酸二甲酯 | 194.18 | 19g | 1.02 | 99% |
| 偏二苯基丙酮 | 210.27 | 20g | 1 | 95% |
| 甲苯 | 92.14 | 250ml | ||
| 水 | 2000ml | |||
| 氢氧化钠 | / |
试验步骤：
1.在干燥的2000毫升容量的三口烧瓶内，通入氮气，来回置换三次，然后加入600毫升浓度为1.6摩尔每升的苯基氯化镁四氢呋喃溶液，然后置于冰水浴中，控制内部温度在0摄氏度左右；
2. 搅拌下，滴加乳酸乙酯-四氢呋喃溶液，乳酸乙酯82.5毫升、四氢呋喃100毫升四氢呋喃，滴加完毕后，撤除冰浴，更换成油浴，缓慢升温至回流温度，回流2小时；
3. 撤除油浴，用冰水冷却至0摄氏度，快速搅拌下滴加10%稀盐酸溶液（约需1.8摩尔，165毫升浓盐酸和400毫升水）；
4. 分液，分出有机层，水相用150毫升二氯甲烷洗涤两次，合并有机相，干燥、浓缩；
5. 在得到的浓缩相内加入20%浓度硫酸（按体积计75毫升浓硫酸+225毫升水），加热到90摄氏度回流3-4小时，分液；
6. 有机相里加水100毫升，用液碱调pH=7、水洗，得到的有机相浓缩得粘稠状产品；
7. 甲醇重结晶，得到白色固体，即偏二苯基丙酮。
二、敌鼠钠盐的制备
试验物料：
| 名 称 | 分子量 | 投料量 | 摩尔比 | 纯度 |
| 甲醇钠 | 54.02 | 21g | 1.3 | 30% |
| 邻苯二甲酸二甲酯 | 194.18 | 19g | 1.02 | 99% |
| 偏二苯基丙酮 | 210.27 | 20g | 1 | 95% |
| 甲苯 | 92.14 | 250ml | ||
| 水 | 2000ml | |||
| 氢氧化钠 | / |
试验步骤：
1.在装有机械搅拌装置的500毫升容量的三口瓶，搭建蒸馏装置；
2. 投甲醇钠21克和100毫升甲苯，搅拌，常压脱甲醇，甲醇脱完，形成乳白色甲醇钠悬浮液，降温至100摄氏度以下；
3. 搅拌下，倒入邻二苯二甲酸二甲酯和甲苯溶液（邻二苯二甲酸二甲酯19克和50毫升甲苯）；
4.升温到内温110摄氏度，缓慢滴加偏二苯基丙酮和甲苯溶液（偏二苯基丙酮20克，100毫升甲苯）大约3-4小时滴加完，控制内温110摄氏度，中途有少量的甲醇蒸出，滴加完后110摄氏度保温1个小时；
5. 降温至80摄氏度，加2%的碱水25毫升，80摄氏度搅拌30分钟，冷却到20摄氏度过滤，滤饼用水漂洗，抽干、干燥，最终得到产品敌鼠钠盐。
以上仅是本发明的具体应用范例，对本发明的保护范围不构成任何限制。凡采用等同变换或者等效替换而形成的技术方案，均落在本发明权利保护范围之内。
Claims (4)
1.一种高效环保敌鼠钠盐制备工艺方法，其特征在于，其合成工艺路线为：
具体包括以下步骤：
步骤一：苯基格氏试剂和乳酸酯反应，生成1,1-二苯基-1，2-丙二醇，即中间体1；
步骤二：将所述步骤一得到的中间体1在硫酸中脱水，合成得到偏二苯基丙酮；
步骤三：将所述步骤一得到的偏二苯基丙酮首先和邻苯二甲酸二甲酯进行缩合，然后用氢氧化钠碱化，最后得到敌鼠钠盐。
2.根据权利要求1所述的一种高效环保敌鼠钠盐制备工艺方法，其特征在于：所述1,1-二苯基-1，2-丙二醇，即中间体1是通过苯基格式试剂和乳酸酯采用格式反应制得的。
3.根据权利要求1所述的一种高效环保敌鼠钠盐制备工艺方法，其特征在于：所述苯基格氏试剂为是苯基氯化镁或者是苯基溴化镁。
4.根据权利要求1所述的一种高效环保敌鼠钠盐制备工艺方法，其特征在于：所述乳酸酯为乳酸乙酯或乳酸甲酯或乳酸丙酯或乳酸异丙酯或乳酸丁酯。
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