CN113620870A - 2-氯烟酸的制备方法及含该2-氯烟酸的杀虫喷雾剂 - Google Patents

2-氯烟酸的制备方法及含该2-氯烟酸的杀虫喷雾剂 Download PDF

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CN113620870A
CN113620870A CN202110801040.6A CN202110801040A CN113620870A CN 113620870 A CN113620870 A CN 113620870A CN 202110801040 A CN202110801040 A CN 202110801040A CN 113620870 A CN113620870 A CN 113620870A
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齐鲲鹏
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Abstract

本发明提供了一种2‑氯烟酸的制备方法及含该2‑氯烟酸的杀虫喷雾剂，其中，2‑氯烟酸通过3‑氰基吡啶的N‑氧化物为原料依次经氯化、碱性水解可得。此制备方法中，以3‑氰基吡啶的N‑氧化物为原料，此原料仅通过3‑氰基吡啶于双氧水的氧化条件下氧化反应即可得，其反应原料易得，且3‑氰基吡啶的N‑氧化物依次经氯化、碱性水解，此两种反应的工艺路线简单，且产品的收率较高，有利于2‑氯烟酸的应用推广。本发明的杀虫喷雾剂，按重量百分比计，制备原料包括2‑氯烟酸1～10％、胡椒基丁醚1～10％、乙二醇0.1～1％和D40溶剂油80～95％，此杀虫喷雾剂的杀虫效果好，且危险系数低。

Description

2-氯烟酸的制备方法及含该2-氯烟酸的杀虫喷雾剂
技术领域
本发明涉及化学试剂合成的技术领域，尤其涉及2-氯烟酸的制备方法及含该2-氯烟酸的杀虫喷雾剂。
背景技术
近年来市场对新型、高效、低用量、安全性好的新农药及高效的新医药的需求越来越大，然而合成这些药物对应的原料却出现了短缺，从而大大制约了新产品的推广和使用，而2-氯烟酸就是其中一种。
2-氯烟酸广泛的应用于医药和农药中，目前2-氯烟酸的合成方法主要有：(1)以烟酸为起始原料经双氧水进行N-氧化、氯化和水解合成2-氯烟酸；(2)2-氯-3-甲基吡啶氧化法；(3)氰基乙酸乙酯为原料的加环法；(4)2-氯-3-三氟甲基吡啶为原料氯化水解法。但是上述合成方法存在各种问题，如方式(1)经过了多个反应，其产率较低，且氯化时容易出现多取代产物，且使用POCl3进行氯化，其使用量过大，也存在大量的废酸污染环境，难以达到环保要求。方式(2)中，其工艺路线简单，反应条件温和，产品的纯度高，但是收率很低，且原料2-氯-3-甲基吡啶很难得，难以实现工业化生产。方式(3)的加环法路线简单，产品选择性高，但是反应时间长，且原料难得，而方式(4)同样存在原料难得及昂贵的问题，且反应产生大量的废酸，难以回收处理，难以进行工业化。
基于此，有必要提供一种新的2-氯烟酸的制备方法，以提高其收率从而满足杀虫喷雾剂的使用要求。
发明内容
本发明的目的之一在于提供一种2-氯烟酸的制备方法的制备方法，通过该方法制备而得的2-氯烟酸的制备方法产率高，合成方式简单，且原料易得。
本发明的目的之二在于提供了一种含2-氯烟酸的杀虫喷雾剂，此杀虫喷雾剂的杀虫效果好，且危险系数低。
为实现上述第一目的，本发明第一方面提供了一种2-氯烟酸的制备方法，通过3-氰基吡啶的N-氧化物为原料依次经氯化、碱性水解可得。
本发明采取的2-氯烟酸的制备方法中，以3-氰基吡啶的N-氧化物为原料，此原料仅通过3-氰基吡啶于双氧水的氧化条件下氧化反应即可得，其反应原料易得。3-氰基吡啶的N-氧化物依次经氯化、碱性水解，此两种反应的工艺路线简单，且产品的收率较高，有利于2-氯烟酸的应用推广。
较佳的，2-氯烟酸的制备方法包括步骤：
(1)氯化反应
利用3-氰基吡啶的N-氧化物和双(三氯甲基)碳酸酯于有机碱的作用下进行氯化反应得2-氯-3-氰基吡啶；
(2)碱性水解
将所述2-氯-3-氰基吡啶于80～90℃的碱性条件下水解。
采用双(三氯甲基)碳酸酯作为氯化剂相当于传统的POCl3、POCl5，其为绿色试剂，对环境污染小不存在废液污染等问题，利于工业化发展。
较佳的，所述有机碱为乙醇胺、乙二胺、二甲胺、三甲胺、三乙胺、丙胺、异丙胺、丙二胺、三丙胺和三乙醇胺中的至少一种，优选为乙醇胺或三乙醇胺。
本发明第二方面提供了一种杀虫喷雾剂，按重量百分比计，制备原料包括2-氯烟酸1～10％、胡椒基丁醚1～10％、乙二醇0.1～1％和D40溶剂油80～95％，所述2-氯烟酸为前述的2-氯烟酸的制备方法所制备的2-氯烟酸。
本发明的制备原料中，本发明采用2-氯烟酸作为杀虫剂的主要药效成分，其具有高效毒性，且具有复杂的分子结构，害虫难以对其产生抗性。胡椒基丁醚可与2-氯烟酸产生复配效果，除了能数十倍地提高2-氯烟酸的杀虫效果还可以延长药效时间，因而通过2-氯烟酸和胡椒基丁醚的结合大大提高了杀虫效果。通过在杀虫剂中加入80～95％的D40溶剂油，D40溶剂油的含量远高于2-氯烟酸和胡椒基丁醚的总含量，因而杀虫剂主要以D40溶剂油的形态而存在，D40溶剂油既可以作为良溶剂以溶解2-氯烟酸和胡椒基丁醚从而使两者更好的分散以实现药效上的复配，同时其优良的挥发性及稀释性可以使杀虫剂不含有抛射剂时从喷雾罐中喷出也能呈现良好的雾化效果，因而大大降低杀虫剂使用时的危险系数。另外，通过加入0.1～1％的乙二醇，乙二醇与D40溶剂油不相溶，因而低含量的乙二醇并不影响D40溶剂油的性能及形态，且低含量的乙二醇其冰点较低可以减少喷雾剂的蒸气压以进一步提高喷雾剂的安全性。
较佳的，杀虫喷雾剂的制备原料包括2-氯烟酸1～5％、胡椒基丁醚3～7％、乙二醇0.1～0.5％、D40溶剂油88～93％和0.01～0.2％的阻燃剂，阻燃剂可防止杀虫喷雾剂在使用时可燃性物质遇到火源时或者温度过高而导致的燃烧。所述阻燃剂为膨胀型助燃剂，膨胀性阻燃剂可释放不可燃气体并把可燃气体的浓度冲淡到燃烧下限以下，稀释燃烧区内的氧浓度，阻止燃烧的继续进行，从而达到阻燃的作用。进一步的，所述阻燃剂为聚磷酰胺或聚磷酸铵，更具体的为聚苯氧基对苯磷酰二胺、聚苯氧基间苯磷酰二胺或聚磷酸铵。因含有磷酰胺结构和磷酸铵结构，含磷量大、含氮量高，磷氮体系产生协同效应，阻燃性好。同时聚苯氧基对苯磷酰二胺、聚苯氧基间苯磷酰二胺和聚磷酸铵在乙二醇中分散性良好。
本发明的第三方面提供了一种杀虫喷雾剂的制备方法，包括如下步骤：
(1)将2-氯烟酸、胡椒基丁醚、乙二醇和D40溶剂油按配比混合，制成药液；
(2)将所述药液注入灌气机，往气雾罐内注入气体并封闭气雾罐口，所述灌气机通过所述气雾罐囗将所述药液灌入所述气雾罐内。
如果制备原料还包括0.01～0.2％的阻燃剂，那么在上述方法中第(1)步将阻燃剂同2-氯烟酸、胡椒基丁醚、乙二醇和D40溶剂油一起混合制成药液，再进行第二步操作。
具体实施方式
本发明的2-氯烟酸的制备采用通过3-氰基吡啶的N-氧化物为原料依次经氯化、碱性水解可得。具体的，包括步骤：
(1)氯化反应
利用3-氰基吡啶的N-氧化物和双(三氯甲基)碳酸酯于有机碱的作用下进行氯化反应得2-氯-3-氰基吡啶；
(2)碱性水解
Figure BDA0003164800730000041
将所述2-氯-3-氰基吡啶于80～90℃的碱性条件下水解。
其整个反应流程为：
通过此合成路线，其反应的工艺路线简单，且产品的收率较高，有利于2-氯烟酸的应用推广。本发明的2-氯烟酸用途较广，可用于农药及医药领域等。由于其具有高效毒性，且具有复杂的分子结构，害虫难以对其产生抗性，因而可用于杀虫剂。为更好地说明本发明的目的、技术方案和有益效果，下面将结合具体实施例对本发明作进一步说明。需说明的是，下述实施所述方法是对本发明做的进一步解释说明，不应当作为对本发明的限制。
实施例1
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸3％、胡椒基丁醚7％、乙二醇0.5％和D40溶剂油89.5％。其具体制备方法为：
包括步骤：
(1)将2-氯烟酸、胡椒基丁醚、乙二醇和D40溶剂油按配比混合，制成药液；
(2)将药液注入灌气机，往喷雾罐内注入气体并封闭喷雾罐口，灌气机通过喷雾罐囗将药液灌入喷雾罐内。
其中，2-氯烟酸通过3-氰基吡啶的N-氧化物为原料依次经氯化、碱性水解可得，具体合成步骤为：
(1)氯化反应
利用3-氰基吡啶的N-氧化物和双(三氯甲基)碳酸酯于三乙醇胺的作用下进行氯化反应得2-氯-3-氰基吡啶；
(2)碱性水解
将2-氯-3-氰基吡啶于80～90℃的碱性条件下水解。
实施例2
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸5％、胡椒基丁醚4.6％、乙二醇0.4％和D40溶剂油90％。其具体制备方法为：
包括步骤：
(1)将2-氯烟酸、胡椒基丁醚、乙二醇和D40溶剂油按配比混合，制成药液；
(2)将药液注入灌气机，往喷雾罐内注入气体并封闭喷雾罐口，灌气机通过喷雾罐囗将药液灌入喷雾罐内。
其中，2-氯烟酸通过3-氰基吡啶的N-氧化物为原料依次经氯化、碱性水解可得，具体合成步骤为：
(1)氯化反应
利用3-氰基吡啶的N-氧化物和双(三氯甲基)碳酸酯于乙醇胺的作用下进行氯化反应得2-氯-3-氰基吡啶；
(2)碱性水解
将2-氯-3-氰基吡啶于80～90℃的碱性条件下水解。
实施例3
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸3％、胡椒基丁醚7％、乙二醇0.5％、D40溶剂油89.4％和聚磷酸铵0.1％。其具体制备方法为：
包括步骤：
(1)将2-氯烟酸、胡椒基丁醚、乙二醇、D40溶剂油和聚磷酸铵按配比混合，制成药液；
(2)将药液注入灌气机，往喷雾罐内注入气体并封闭喷雾罐口，灌气机通过喷雾罐囗将药液灌入喷雾罐内。
其中，2-氯烟酸的制备方法同实施例1。
实施例4
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸7％、胡椒基丁醚5％、乙二醇0.2％、D40溶剂油87.6％和聚苯氧基对苯磷酰二胺0.2％。其具体制备方法及2-氯烟酸的制备方法同实施例1。
对比例1
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸10％、乙二醇0.5％和D40溶剂油89.5％。其具体制备方法及2-氯烟酸的制备方法同实施例1。
对比例2
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸3％、胡椒基丁醚7％和D40溶剂油90％。其具体制备方法及2-氯烟酸的制备方法同实施例1。
对比例3
一种杀虫喷雾剂的制备原料，按重量百分比计，包括2-氯烟酸3％、胡椒基丁醚7％、乙二醇0.5％和乙醇89.5％。其具体制备方法及2-氯烟酸的制备方法同实施例1。
将实施例1～4、对比例1～3的杀虫喷雾剂通过如下测试验证其杀虫效果，其结果如表3所示。
测试方法：
在一间30立方米的房间内安装一个自动喷雾器及杀虫喷雾剂，自动喷雾器安装在2米高的墙上，将程式调至每4min喷一次，每次喷出的剂量为30mg。然后将100只蚊子和苍蝇放入房间，每5-15min会观察房间内的蚊子及苍蝇的死亡率直到90min。
表3实施例1～4、对比例1～3的杀虫喷雾剂的杀虫效果
Figure BDA0003164800730000071
从表3可知，实施例1～4的杀虫效果要好于对比例1～3，主要由于本发明中杀虫喷雾剂的制备原料通过2-氯烟酸1～10％、胡椒基丁醚1～10％、乙二醇0.1～1％和D40溶剂油80～95％进行结合，80～95％％的D40溶剂油既可以作为良溶剂以溶解2-氯烟酸和胡椒基丁醚从而使两者实现药效上的复配，同时其优良的挥发性及稀释性可以使杀虫剂呈现良好的雾化效果，因而能在房间内快速的分散到室内每个角落，并会将室内的蚊虫杀死。
对比实施例1～4可知，制备原料中加入阻燃剂之后，其杀虫效果更佳，可能与其释放不可燃气体相关。
最后应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，但是也并不仅限于实施例中所列，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

1.一种2-氯烟酸的制备方法，其特征在于，通过3-氰基吡啶的N-氧化物为原料依次经氯化、碱性水解可得。
2.根据权利要求1所述的2-氯烟酸的制备方法，其特征在于，包括步骤：
(1)氯化反应
利用3-氰基吡啶的N-氧化物和双(三氯甲基)碳酸酯于有机碱的作用下进行氯化反应得2-氯-3-氰基吡啶；
(2)碱性水解
将所述2-氯-3-氰基吡啶于80～90℃的碱性条件下水解。
3.根据权利要求2所述的2-氯烟酸的制备方法，其特征在于，所述有机碱为乙醇胺、乙二胺、二甲胺、三甲胺、三乙胺、丙胺、异丙胺、丙二胺、三丙胺和三乙醇胺中的至少一种。
4.一种杀虫喷雾剂，其特征在于，按重量百分比计，制备原料包括2-氯烟酸1～10％、胡椒基丁醚1～10％、乙二醇0.1～1％和D40溶剂油80～95％，所述2-氯烟酸为权利要求1～3任一所述的2-氯烟酸的制备方法所制备的2-氯烟酸。
5.根据权利要求4所述的杀虫喷雾剂，其特征在于，按重量百分比计，制备原料包括2-氯烟酸1～5％、胡椒基丁醚3～7％、乙二醇0.1～0.5％和D40溶剂油88～93％。
6.根据权利要求4所述的杀虫喷雾剂，其特征在于，还包括0.01～0.2％的阻燃剂。
7.根据权利要求6所述的杀虫喷雾剂，其特征在于，所述阻燃剂为膨胀型助燃剂。
8.根据权利要求7所述的杀虫喷雾剂，其特征在于，所述阻燃剂为聚磷酰胺或聚磷酸铵。
9.根据权利要求8所述的杀虫喷雾剂，其特征在于，所述阻燃剂为聚苯氧基对苯磷酰二胺、聚苯氧基间苯磷酰二胺或聚磷酸铵。
10.根据权利要求4～9任一所述的杀虫喷雾剂的制备方法，其特征在于，包括步骤：
(1)将2-氯烟酸、胡椒基丁醚、乙二醇和D40溶剂油按配比混合，制成药液；
(2)将所述药液注入灌气机，往喷雾罐内注入气体并封闭喷雾罐口，所述灌气机通过所述喷雾罐囗将所述药液灌入所述喷雾罐内。
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CN111393361A (zh) * 2019-12-30 2020-07-10 浙江日出药业有限公司 一种安全环保的2-氯烟酸合成方法
CN112375035A (zh) * 2020-12-11 2021-02-19 菲立化学工程(遂昌)有限公司 一种制备2-氯烟酸的连续化反应系统及方法

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CN111393361A (zh) * 2019-12-30 2020-07-10 浙江日出药业有限公司 一种安全环保的2-氯烟酸合成方法
CN112375035A (zh) * 2020-12-11 2021-02-19 菲立化学工程(遂昌)有限公司 一种制备2-氯烟酸的连续化反应系统及方法

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