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WO2018039843A1 - Procédé de préparation de glyphosate - Google Patents

Procédé de préparation de glyphosate 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
Authority
WO
WIPO (PCT)
Prior art keywords
added
solution
stirring
catalyst
glyphosate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2016/097094
Other languages
English (en)
Chinese (zh)
Inventor
沈建美
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to PCT/CN2016/097094 priority Critical patent/WO2018039843A1/fr
Publication of WO2018039843A1 publication Critical patent/WO2018039843A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77Heterocyclic 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
    • C07D307/78Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/79Benzo [b] furans; Hydrogenated benzo [b] furans with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the hetero ring
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77Heterocyclic 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
    • C07D307/78Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/79Benzo [b] furans; Hydrogenated benzo [b] furans with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the hetero ring
    • C07D307/80Radicals substituted by oxygen atoms
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77Heterocyclic 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
    • C07D307/78Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/82Benzo [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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77Heterocyclic 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
    • C07D307/78Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/82Benzo [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
    • C07D307/84Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen
    • C07D307/85Carbon 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

L'invention concerne un procédé de préparation de glyphosate. Tout d'abord, un composé substitué en 2-halogène et un composé ortho-hydroxy sont successivement ajoutés à un solvant sous agitation, et après agitation uniforme, une solution alcaline est ensuite ajoutée, et le mélange est placé à une température de 200 °C et mis à réagir pendant 1 heure; la solution est refroidie à température ambiante et un catalyseur est ajouté, et une réaction catalytique est effectuée pendant 30 minutes; et enfin, l'acide chlorhydrique est ensuite ajouté à la solution et agité à une vitesse élevée pour effectuer une décarboxylation d'acidification pendant 0,5 h, et la vitesse d'agitation est réglée à 500 r/min. Les avantages résident en ce que le composé substitué en 2-halogène et le composé ortho-hydroxy sont utilisés en tant que matières premières de préparation, les matières premières sont peu coûteuses et facilement obtenues; le temps de réaction est court, l'opération est simple, le produit est facilement purifié, aucun catalyseur précieux n'est utilisé, le rendement est élevé et la pollution est faible.
PCT/CN2016/097094 2016-08-29 2016-08-29 Procédé de préparation de glyphosate Ceased WO2018039843A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2016/097094 WO2018039843A1 (fr) 2016-08-29 2016-08-29 Procédé de préparation de glyphosate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2016/097094 WO2018039843A1 (fr) 2016-08-29 2016-08-29 Procédé de préparation de glyphosate

Publications (1)

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

Family

ID=61299693

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2016/097094 Ceased WO2018039843A1 (fr) 2016-08-29 2016-08-29 Procédé de préparation de glyphosate

Country Status (1)

Country Link
WO (1) WO2018039843A1 (fr)

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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