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1. WO2022134385 - PURIFICATION METHOD FOR 4"-(S)-METHYLAMINO ABAMECTIN B2A BENZOATE

Publication Number WO/2022/134385
Publication Date 30.06.2022
International Application No. PCT/CN2021/086469
International Filing Date 12.04.2021
IPC
C07H 1/06 2006.1
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
1Processes for the preparation of sugar derivatives
06Separation; Purification
C07H 17/08 2006.1
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
17Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
04Heterocyclic radicals containing only oxygen as ring hetero atoms
08Hetero rings containing eight or more ring members, e.g. erythromycins
C07C 63/08 2006.1
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
63Compounds having carboxyl groups bound to carbon atoms of six-membered aromatic rings
04Monocyclic monocarboxylic acids
06Benzoic acid
08Salts thereof
C07C 51/43 2006.1
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
51Preparation of carboxylic acids or their salts, halides, or anhydrides
42Separation; Purification; Stabilisation; Use of additives
43by change of the physical state, e.g. crystallisation
CPC
C07C 51/43
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
51Preparation of carboxylic acids or their salts, halides or anhydrides
42Separation; Purification; Stabilisation; Use of additives
43by change of the physical state, e.g. crystallisation
C07C 63/08
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
63Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
04Monocyclic monocarboxylic acids
06Benzoic acid
08Salts thereof
C07H 1/06
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
1Processes for the preparation of sugar derivatives
06Separation; Purification
C07H 17/08
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
17Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
04Heterocyclic radicals containing only oxygen as ring hetero atoms
08Hetero rings containing eight or more ring members, e.g. erythromycins
Applicants
  • 河北威远生物化工有限公司 HEBEI VEYONG BIO-CHEMICAL CO., LTD [CN]/[CN]
Inventors
  • 王博 WANG, Bo
  • 田学芳 TIAN, Xuefang
  • 高永民 GAO, Yongmin
  • 张博 ZHANG, Bo
  • 张丽荣 ZHANG, Lirong
  • 李志峰 LI, Zhifeng
  • 李立华 LI, Lihua
  • 范朝辉 FAN, Zhaohui
  • 贾成国 JIA, Chengguo
Agents
  • 河北国维致远知识产权代理有限公司 HEBEI GUOWEIZHIYUAN INTELLECTUAL PROPERTY AGENCY CO., LTD
Priority Data
202011568862.625.12.2020CN
Publication Language Chinese (zh)
Filing Language Chinese (ZH)
Designated States
Title
(EN) PURIFICATION METHOD FOR 4"-(S)-METHYLAMINO ABAMECTIN B2A BENZOATE
(FR) PROCÉDÉ DE PURIFICATION DE BENZOATE DE 4"-(S)-MÉTHYLAMINO ABAMECTINE B2A
(ZH) 一种4"-(s)-甲氨基阿维菌素B2a苯甲酸盐的纯化方法
Abstract
(EN) The present invention relates to the technical field of agricultural chemicals and preparation. Specifically, disclosed is a purification method for 4"-(s)-methylamino abamectin B2a benzoate. The purification method comprises the following steps: adding a crude product of methylamino abamectin B2a/2b benzoate to methyl tert-butyl ether, heating and dissolving, dropwise adding a mixed solution of tert-butanol and n-butyl ether, cooling and filtering after the dropwise adding, and cooling and crystallizing an obtained filtrate to obtain a product of 4"-(s)-methylamino abamectin B2a benzoate. According to the purification method provided by the present invention, by selecting the mixed solution of methyl tert-butyl ether, tert-butanol and n-butyl ether as a crystallization solvent, and in coordination with twice cooling and crystallization, the product of 4"-(s)-methylamino abamectin B2a benzoate having S-configured methylamino at bit 4" and having a content of 98% or more is obtained, thereby facilitating improvement of the insecticidal activity of related preparations, and achieving a wide application prospect.
(FR) La présente invention relève du domaine technique des produits agrochimiques et de la préparation. L'invention concerne en particulier un procédé de purification de benzoate de 4"-(s)-méthylamino abamectine B2a. Le procédé de purification comprend les étapes suivantes consistant à : ajouter un produit brut de benzoate de méthylamino abamectine B2a/2b à l'éther de tert-butylméthylique, faire chauffer et dissoudre, ajouter goutte à goutte une solution mixte d'éther de tert-butanol et de n-butyle, refroidir et filtrer après l'ajout goutte à goutte, et refroidir et cristalliser un filtrat obtenu pour obtenir un produit de benzoate de 4"-(s)-méthylamino abamectine B2a. Le procédé de purification fourni par la présente invention est basé sur la sélection d'une solution mixte d'éther de tert-butylméthylique, de tert-butanol et d'éther de n-butyle comme solvant de cristallisation, et la coordination avec le double refroidissement et la cristallisation, ce qui permet d'obtenir un produit de benzoate de 4"-(s)-méthylamino abamectine B2a ayant du méthylamino S-configuré à 4" bit et ayant une teneur de 98 % ou plus, ce qui facilite l'amélioration de l'activité insecticide de préparations apparentées, et permet d'obtenir une large perspective d'application.
(ZH) 本方案涉及农用化学品及制备技术领域,具体公开一种4"-(s)-甲氨基阿维菌素B2a苯甲酸盐的纯化方法。所述纯化方法包括以下步骤:将甲氨基阿维菌素B2a/2b苯甲酸盐粗品加入甲基叔丁基醚中,加热溶解,然后滴加叔丁醇和正丁醚混合溶液,滴加结束后降温过滤,将所得滤液降温析晶,得到4"-(s)-甲氨基阿维菌素B2a苯甲酸盐产品。本方案提供的纯化方法,通过选择甲基叔丁基醚、叔丁醇和正丁醚的混合溶液作为结晶溶剂,并配合两次降温析晶的方式,得到4"位甲胺基为s构型、含量98%以上的4"-(s)-甲氨基阿维菌素B2a苯甲酸盐产品,有利于提高其相关制剂的杀虫活性,具有广阔的应用前景。
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