WO2018039845A1 - Procédé de préparation d'anhydride hydroxybenzoïque - Google Patents

Procédé de préparation d'anhydride hydroxybenzoïque Download PDF

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Publication number
WO2018039845A1
WO2018039845A1 PCT/CN2016/097106 CN2016097106W WO2018039845A1 WO 2018039845 A1 WO2018039845 A1 WO 2018039845A1 CN 2016097106 W CN2016097106 W CN 2016097106W WO 2018039845 A1 WO2018039845 A1 WO 2018039845A1
Authority
WO
WIPO (PCT)
Prior art keywords
anhydride
benzoic
hydroxybenzoic
preparing
preparation
Prior art date
Application number
PCT/CN2016/097106
Other languages
English (en)
Chinese (zh)
Inventor
沈建美
Original Assignee
沈建美
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 沈建美 filed Critical 沈建美
Priority to PCT/CN2016/097106 priority Critical patent/WO2018039845A1/fr
Publication of WO2018039845A1 publication Critical patent/WO2018039845A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/54—Preparation of carboxylic acid anhydrides
    • C07C51/56—Preparation of carboxylic acid anhydrides from organic acids, their salts, their esters or their halides, e.g. by carboxylation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/04—Monocyclic monocarboxylic acids
    • C07C63/06—Benzoic acid

Definitions

  • the invention belongs to the technical field of preparation of organic compounds, and in particular relates to a preparation method of hydroxybenzoic anhydride.
  • Hydroxybenzoic anhydride is a commonly used organic intermediate and has a wide range of uses in organic synthesis, chemical raw materials, pharmaceutical preparation, etc., especially in the pharmaceutical industry as a basic intermediate to derive a large number of organic compounds and new varieties. Commonly used for the determination of water. Benzoic acid liver is formed by the condensation of benzoic acid with acetic anhydride. Benzoic anhydride, also known as benzoic anhydride, is a colorless orthorhombic prism crystal, insoluble in water, soluble in ether and ethanol, stable to water and cold alkali, and can be hydrolyzed by boiling alkali metal carbonates and caustic. The preparation of common benzoic anhydride is low in purity and cannot be used by people.
  • the object of the present invention is to provide a method for preparing benzoic anhydride having high purity and high quality in view of the deficiencies of the prior art.
  • the technical solution of the present invention is: a method for preparing benzoic anhydride, which is innovative in that the steps are as follows:
  • fractional distillation under reduced pressure, and fractions below 145 ° C, 145-175 ° C, and 175-200 ° C are separately collected at 15-19 mmHg, the latter being a crude benzoic anhydride, a lower temperature fraction and the above
  • the fractions of 120-130 °C are combined, and after adding a drop of phosphoric acid, fractional distillation is carried out to obtain some 210-220/20 mmHg fractions, ie crude benzoic anhydride, total crude product 1.0-1.2 Kg, normal pressure 120-130 °C
  • the fraction is subjected to re-distillation to obtain crude acetic acid below 120 ° C and crude acetic anhydride at 130-140 ° C;
  • the preparation method of the benzoic anhydride of the invention is simple and easy to operate, convenient to operate, easy to obtain raw materials, common in equipment, short in cycle and high in purity.
  • a method for preparing hydroxybenzoic anhydride the steps are as follows:
  • the preparation method of the invention adopts benzoic anhydride, which is simple and easy to operate, convenient to operate, easy to obtain raw materials, common in equipment, short in cycle and high in purity.

Abstract

L'invention concerne un procédé de préparation d'anhydride hydroxybenzoïque. L'acide benzoïque et l'anhydride acétique sont placés dans un récipient, un mélange réactionnel est lentement distillé pour obtenir un produit d'anhydride hydroxybenzoïque pur, et une liqueur mère ayant un point de fusion de 50°C est concentrée dans un bain d'eau et recristallise à nouveau, de telle sorte qu'un produit pur est obtenu. Les avantages résident dans le fait que le procédé de préparation utilisant de l'anhydride benzoïque est simple et facile à mettre en oeuvre, pratique à utiliser, les matières premières sont facilement disponibles, l'équipement est commun, le cycle est court et la pureté est élevée.
PCT/CN2016/097106 2016-08-29 2016-08-29 Procédé de préparation d'anhydride hydroxybenzoïque WO2018039845A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2016/097106 WO2018039845A1 (fr) 2016-08-29 2016-08-29 Procédé de préparation d'anhydride hydroxybenzoïque

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2016/097106 WO2018039845A1 (fr) 2016-08-29 2016-08-29 Procédé de préparation d'anhydride hydroxybenzoïque

Publications (1)

Publication Number Publication Date
WO2018039845A1 true WO2018039845A1 (fr) 2018-03-08

Family

ID=61299709

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2016/097106 WO2018039845A1 (fr) 2016-08-29 2016-08-29 Procédé de préparation d'anhydride hydroxybenzoïque

Country Status (1)

Country Link
WO (1) WO2018039845A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1222131A (zh) * 1996-06-20 1999-07-07 罗狄亚化学公司 芳族化合物的酰化方法
CN1249737A (zh) * 1997-03-12 2000-04-05 罗狄亚化学公司 芳族化合物的酰化或磺酰化方法
CN104130121A (zh) * 2014-07-14 2014-11-05 天津市化学试剂研究所有限公司 苯甲酸酐的制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1222131A (zh) * 1996-06-20 1999-07-07 罗狄亚化学公司 芳族化合物的酰化方法
CN1249737A (zh) * 1997-03-12 2000-04-05 罗狄亚化学公司 芳族化合物的酰化或磺酰化方法
CN104130121A (zh) * 2014-07-14 2014-11-05 天津市化学试剂研究所有限公司 苯甲酸酐的制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZHANG GUANLI ET AL.: "The synthesis of 4-cyan-o-phthalic anhydride", NEW CHEMICAL MATERIALS, vol. 7, no. 30, 31 July 2002 (2002-07-31), pages 34 - 35 *

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