专利号:WO-2022099693-A1 优先权日:2020-11-16 标题 :Method for improving effect of fluorination reaction in synthesis of 2-chloro-5-trifluoromethyl pyridine, and matching system 发明人:ZHA ZHIXIONG; LI HAO 权利人:SHANXIAN XINRUN CHEMICAL CO LTD 摘要:The present invention relates to the technical field of chemical synthesis, and particularly, a method for improving effect of fluorination reaction in the synthesis of 2-chloro-5-trifluoromethyl pyridine, and a matching system. The method comprises the following steps: preparing 2-chloro-5-trichloromethyl pyridine, and adding to an efficient reaction system after superfine crushing; adding an appropriate amount of iodine pentafluoride, mercury fluoride and a catalyst into the efficient reaction system; controlling the temperature and time, and carrying out a fluorination reaction on materials in the high-pressure, sealed, efficient reaction system to obtain a crude solution containing 2-chloro-5-trifluoromethyl pyridine; purifying the above crude solution to obtain 2-chloro-5-trifluoromethyl pyridine. In the present method, a fluorination reaction is carried out in a high-pressure sealed environment, such that the efficiency and effect of the fluorination reaction are effectively improved. By means of the system in the present invention, the material entering the system may be quickly superfine crushed before the reaction, so as to improve the reaction sufficiency in the subsequent reaction process.
专利号:US-4658031-A 优先权日:1982-10-07 标 题:Synthesis of 2-substituted-5-methyl-pyridines and intermediates therefor 发明人:HARTMANN LUDWIG A; STEPHEN JOHN F 权利人:ICI AMERICA INC 摘要:A process for the synthesis of compounds which are known intermediates for the pyridyloxyphenoxy herbicies as well as intermediates used in the process. Propionaldehyde and an acrylic compound, two readily available starting materials, are reacted to form a 2-formylpentanoic compound which is cyclized to a dihydro pyridone which is then oxidized to the 2-hydroxy pyridine. The hydroxypyridine may be halogenated to a 2-halopyridine.
专利号:US-4584380-A 优先权日:1982-10-07 标 题:Synthesis of 2-substituted-5-methyl-pyridines and intermediates therefor 发明人:HARTMANN LUDWIG A; STEPHEN JOHN F 权利人:ICI AMERICA INC 摘要:A process for the synthesis of compounds which are known intermediates for the pyridyloxyphenoxy herbicides as well as intermediates used in the process. Propionaldehyde and an acrylic compound, two readily available starting materials, are reacted to form a 2-formylpentanoic compound which is cyclized to a dihydro pyridone which is then oxidized to the 2-hydroxy pyridine. The hydroxypyridine may be halogenated to a 2-halopyridine.
专利号:US-4473696-A 优先权日:1982-10-07 标题:Synthesis of 2-substituted-5-methyl-pyridines 发明人:HARTMANN LUDWIG A; STEPHEN JOHN F 权利人:ICI AMERICA INC 摘要:A process for the synthesis of compounds which are known intermediates for the pyridyloxyphenoxy herbicides as well as intermediates used in the process. Propionaldehyde and an acrylic compound, two readily available starting materials, are reacted to form a 2-formylpentanoic compound which is cyclized to a dihydro pyridone which is then oxidized to the 2-hydroxy pyridine. The hydroxypyridine may be halogenated to a 2-halopyridine.
专利号:US-4687854-A 优先权日:1982-10-07 标 题 :Bispiperidone precursor of 2-substituted-5-methyl-pyridines 发明人:HARTMANN LUDWIG A; STEPHEN JOHN F 权利人:ICI AMERICA INC 摘要:A process for the synthesis of compounds which are known intermediates for the pyridyloxyphenoxy herbicides as well as intermediates used in the process. Propionaldehyde and an acrylic compound, two radily available starting materials, are reacted to form a 2-formylpentanoic compound which is cyclized to a dihydro pyridone which is then oxidized to the 2-hydroxy pyridine. The hydroxypyridine may be halogenated to a 2-halopyridine.
专利号:US-4612377-A 优先权日:1983-03-30 标题:Preparation of 2-chloro-5-methylpyridine 发明人:OSBORNE ROBERT; BAILEY KEVIN D 权利人:ICI PLC 摘要:A 2-oxo-5-methyl-5,6-dihalopiperidine is contacted in a high boiling solvent, preferably trichlorobenzene, with a stoichiometric excess, up to 70 mole % excess, of a chlorinating agent, preferably phosphorus oxychloride or phosgene, at an elevated temperature between 80 DEG and 130 DEG C. The solution of 2-chloro-5-methylpyridine so obtained may be used directly for further chlorination to form 2-chloro-5-trichloromethylpyridine with, for example, chlorine gas in the presence of a free radical initiator. This chemical intermediate is useful in the synthesis of certain herbicidal compounds.
参考标题:Phpocl2 As A Potent Catalyst For Chlorination Reaction Of Phenols With Pcl5 作者:Jiang Wu,Junpeng Zhou,Yalei Shi,Jintao Zhu |发布日期:2016.10.1 摘要:Abstract Phenols Are Easily Converted To The Corresponding Aryl Chlorides By Using Phosphorus Pentachloride (Pcl5) And A Catalytic Amount Of Phenylphosphonic Dichloride (Phpocl2), Which Is A New Efficient Method For Synthesis Of Aryl Chloride In Good Yields. Graphical Abstract