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WO2018039843A1 - 草甘膦的制备工艺 - Google Patents

草甘膦的制备工艺 Download PDF

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Publication number
WO2018039843A1
WO2018039843A1 PCT/CN2016/097094 CN2016097094W WO2018039843A1 WO 2018039843 A1 WO2018039843 A1 WO 2018039843A1 CN 2016097094 W CN2016097094 W CN 2016097094W WO 2018039843 A1 WO2018039843 A1 WO 2018039843A1
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WIPO (PCT)
Prior art keywords
added
solution
stirring
catalyst
glyphosate
Prior art date
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Ceased
Application number
PCT/CN2016/097094
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English (en)
French (fr)
Inventor
沈建美
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Individual
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Individual
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Priority to PCT/CN2016/097094 priority Critical patent/WO2018039843A1/zh
Publication of WO2018039843A1 publication Critical patent/WO2018039843A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/79—Benzo [b] furans; Hydrogenated benzo [b] furans with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the hetero ring
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/79—Benzo [b] furans; Hydrogenated benzo [b] furans with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the hetero ring
    • C07D307/80—Radicals substituted by oxygen atoms
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/82—Benzo [b] furans; Hydrogenated benzo [b] furans with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/82—Benzo [b] furans; Hydrogenated benzo [b] furans with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
    • C07D307/84—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen
    • C07D307/85—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen attached in position 2

Definitions

  • the invention relates to a preparation process of glyphosate, and belongs to the field of chemical processing.
  • Phenylpropanol is an important pharmaceutical and chemical intermediate. It is the backbone of many natural products and drugs. It is the core structure of many medicines and many new drugs currently under development.
  • the preparation of the prior art 1% glyphosate has the following disadvantages: (1) the preparation of raw materials is expensive and the required cost is high; (2) the preparation process is complicated and the work efficiency is low; (3) the preparation of raw materials is difficult, the separation is difficult, and the production is difficult. The rate is lowered; therefore, there is an urgent need to develop a low-cost and high-efficiency 1% glyphosate preparation process, and no technical solutions identical or similar to the present invention have been found by searching.
  • the technical problem to be solved by the present invention is to provide a process for preparing 1% glyphosate which is low in cost and high in production efficiency.
  • the technical solution of the present invention is: a preparation process of glyphosate, and the innovation is as follows: the preparation process is as follows:
  • the 2-halogen substitute and the o-hydroxyl are used as raw materials for preparation, and the raw material is cheap and easy to obtain, and the reaction time is short, the operation is simple, the product is easy to be purified, the noble catalyst is not used, the yield is high, and the pollution is small.
  • the invention discloses a preparation process of glyphosate, and the preparation process is as follows:
  • the 2-halogen substituent and the o-hydroxyl group are sequentially added to the solvent while stirring, and after stirring uniformly, potassium carbonate is added and placed at a temperature of 150 ° C for 2 h; wherein the 2-halogen substituent and the o-hydroxy group are present.
  • the ratio of solvent and potassium carbonate is 1:1:10:10.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

一种草甘膦的制备工艺，首先将2-卤素取代物及邻羟基物依次边搅拌边加入溶剂中，搅拌均匀后再加入碱溶液并放置在200℃的温度下反应1h；将溶液降至室温并加入催化剂，催化反应30min；最后再向溶液中加入盐酸并高速搅拌，使其酸化脱羧0.5h，搅拌速度控制为500r/min。优点在于：采用2-卤素取代物及邻羟基物作为制备原料，该原料便宜易得，同时反应时间短，操作简单，产品容易纯化，不用贵重催化剂，产率高，污染小。

Description

草甘膦的制备工艺 草甘膦的制备工艺
技术领域
本发明涉及草甘膦的制备工艺，属于化学物品加工领域。
背景技术
苯丙呋喃是一种重要的医药化工中间体，是许多天然产物，药物的结构主体骨架，是多种医药以及许多目前正在开发新药的核心结构。
现有技术的1%草甘膦的制备存在以下缺点：（1）制备原料价格昂贵，所需成本高；（2）制备过程繁杂，工作效率低；（3）原料制备困难，分离困难，产率下降；因此急需研制一种成本低且生产效率高的1%草甘膦的制备工艺，经检索，未发现与本发明相同或相似的技术方案。
发明内容
本发明要解决的技术问题是提供一种成本低且生产效率高的1%草甘膦的制备工艺。
为解决上述技术问题，本发明的技术方案为：一种草甘膦的制备工艺，其创新点在于：所述制备工艺具体如下：
（1）将2-卤素取代物及邻羟基物依次边搅拌边加入溶剂中，搅拌均匀后再加入碱溶液并放置在200℃的温度下反应1h；
（2）将溶液降至室温并加入催化剂，催化反应30min；
（3）再向溶液中加入盐酸并高速搅拌，使其酸化脱羧0.5h，搅拌速度控制为500r/min。
本发明的优点在于：
（1）采用2-卤素取代物及邻羟基物作为制备原料，该原料便宜易得，同时反应时间短，操作简单，产品容易纯化，不用贵重催化剂，产率高，污染小。
（2）反应过程中加入二氧化锰催化剂，加快反应速度，提高生产效率。
具体实施方式
实施例1
本发明公开了一种草甘膦的制备工艺，该制备工艺具体如下：
（1）将2-卤素取代物及邻羟基物依次边搅拌边加入溶剂中，其搅拌均匀后再加入碳酸钾并放置在150℃的温度下反应2h；其中2-卤素取代物、邻羟基物、溶剂及碳酸钾的配置比例为1:1:10:10。
（2）将溶液降至室温并加入二氧化锰，催化反应45min；
（3）再向溶液中加入盐酸并高速搅拌，使其酸化脱羧0.5h，搅拌速度控制为500r/min。
以上显示和描述了本发明的基本原理和主要特征。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (1)

  1. 一种草甘膦的制备工艺，其特征在于：所述制备工艺具体如下：
    （1）将2-卤素取代物及邻羟基物依次边搅拌边加入溶剂中，搅拌均匀后再加入碱溶液并放置在200℃的温度下反应1h；
    （2）将溶液降至室温并加入催化剂，催化反应30min；
    （3）再向溶液中加入盐酸并高速搅拌，使其酸化脱羧0.5h，搅拌速度控制为500r/min。
PCT/CN2016/097094 2016-08-29 2016-08-29 草甘膦的制备工艺 Ceased WO2018039843A1 (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2016/097094 WO2018039843A1 (zh) 2016-08-29 2016-08-29 草甘膦的制备工艺

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2016/097094 WO2018039843A1 (zh) 2016-08-29 2016-08-29 草甘膦的制备工艺

Publications (1)

Publication Number Publication Date
WO2018039843A1 true WO2018039843A1 (zh) 2018-03-08

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PCT/CN2016/097094 Ceased WO2018039843A1 (zh) 2016-08-29 2016-08-29 草甘膦的制备工艺

Country Status (1)

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WO (1) WO2018039843A1 (zh)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5364880A (en) * 1993-06-16 1994-11-15 Advanced Therapies, Inc. Compound for treatment of cardiac arrhythmia, synthesis, and methods of use
CN1858042A (zh) * 2006-06-09 2006-11-08 赵金浩 2－丁基－3－(4－羟基－3，5－二碘苯甲酰)苯骈呋喃的合成工艺
CN101830872A (zh) * 2010-04-14 2010-09-15 南方医科大学 一种3-羟基苯并呋喃类衍生物的合成方法
CN102653529A (zh) * 2011-10-25 2012-09-05 广东医学院 一种苯并呋喃的制备工艺
CN104628686A (zh) * 2015-01-27 2015-05-20 南通恒盛精细化工有限公司 一种带酰胺侧链的苯并呋喃制备工艺

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5364880A (en) * 1993-06-16 1994-11-15 Advanced Therapies, Inc. Compound for treatment of cardiac arrhythmia, synthesis, and methods of use
CN1858042A (zh) * 2006-06-09 2006-11-08 赵金浩 2－丁基－3－(4－羟基－3，5－二碘苯甲酰)苯骈呋喃的合成工艺
CN101830872A (zh) * 2010-04-14 2010-09-15 南方医科大学 一种3-羟基苯并呋喃类衍生物的合成方法
CN102653529A (zh) * 2011-10-25 2012-09-05 广东医学院 一种苯并呋喃的制备工艺
CN104628686A (zh) * 2015-01-27 2015-05-20 南通恒盛精细化工有限公司 一种带酰胺侧链的苯并呋喃制备工艺

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