18368-64-4Relevant academic research and scientific papers
Method for preparing 2-chloro-5-substituted pyridine
-
Paragraph 0015; 0061-0064; 0065; 0068, (2021/09/21)
The invention belongs to the technical field of chemical synthesis of pesticides, and particularly relates to a method for preparing 2-chloro-5-substituted pyridine, in particular to a method for preparing 2-chloro-5-methylpyridine. The method comprises the following steps: reacting amide as shown in a formula C which is used as a raw material in the presence of a chlorinating agent and N, N-dimethylformamide, and distilling after the reaction is finished to obtain the 5-substituted 2-chloropyridine as shown in a formula I which is described in the specification. When the 5-substituted 2-chloropyridine is prepared from the compound with the structure shown in the formula C, the by-product is allyl chloride (or homologues thereof) with small molecular weight, the boiling point of the by-product is obviously different from that of the product, the reaction conversion rate and the yield are higher than those of the prior art, the by-product is easy to separate from the product, and the by-product is more beneficial to recovery; therefore, according to the preparation method, the equipment investment can be greatly saved, the production cost is reduced, and the operation procedure is simplified; and in the route, the amine with lower price is used as a starting raw material, so that the production cost is reduced.
Efficient Phosphorus-Free Chlorination of Hydroxy Aza-Arenes and Their Application in One-Pot Pharmaceutical Synthesis
Wang, Jian,Li, Yan-Hui,Pan, Song-Cheng,Li, Ming-Fang,Du, Wenting,Yin, Hong,Li, Jing-Hua
supporting information, p. 146 - 153 (2020/03/10)
The chlorination of hydroxy aza-arenes with bis(trichloromethyl) carbonate (BTC) and SOCl2 has been effectively performed by refluxing with 5 wt % 4-dimethylaminopyridine (DMAP) as a catalyst. Various substrates are chlorinated with high yields. The obtained chlorinated aza-arenes can be used directly with simple workup for succedent one-pot synthesis on a large scale.
A process for preparing 2 - chloro -5 - methyl pyridine method (by machine translation)
-
Paragraph 0012; 0017; 0020, (2019/07/04)
The invention belongs to the technical field of organic chemical industry, relates to 2 - chloro - 5 - methyl pyridine preparation method, more specifically, relates to a 5 - methyl - 3, 4 - dihydro pyridine - 2 (1 H) - one (hereinafter referred to as the: pyridone) and chlorine gas, first synthesis of 2 - hydroxy - 5 - methyl pyridine (hereinafter referred to as: synthetic azo), re-chlorinated preparing 2 - chloro - 5 - methyl pyridine. (by machine translation)
Transition-metal-free decarboxylative halogenation of 2-picolinic acids with dihalomethane under oxygen conditions
Zhang, Xitao,Feng, Xiujuan,Zhang, Haixia,Yamamoto, Yoshinori,Bao, Ming
supporting information, p. 5565 - 5570 (2019/10/22)
A convenient and efficient method for the synthesis of 2-halogen-substituted pyridines is described. The decarboxylative halogenation of 2-picolinic acids with dihalomethane proceeded smoothly via N-chlorocarbene intermediates to afford 2-halogen-substituted pyridines in satisfactory to excellent yields under transition-metal-free conditions. This new type of decarboxylative halogenation is operationally simple and exhibits high functional-group tolerance.
Preparation method of 2-chloro-5-methylpyridine
-
Page/Page column 6-11, (2019/09/17)
The invention provides a preparation method of 2-chloro-5-methylpyridine. The preparation method comprises the following steps: S1, mixing raw materials, including 5-methyl-3,4-dihydro-2(1H)-pyridone,a catalyst and a solvent, to obtain a mixed solution; S2, simultaneously introducing chlorine gas and a chlorinating agent into the mixed solution at a reaction temperature higher than the room temperature, and reacting to obtain a reaction solution containing the 2-chloro-5-methylpyridine. Due to simultaneous introduction of the chlorine gas and the chlorinating agent for a reaction in the method, a technological process of lowering the temperature and then raising the temperature is not required and the 2-chloro-5-methylpyridine is synthesized by a one-step method only, so that the technological process is simplified, and the technological complexity is reduced and can be relatively simple; in addition, experiments indicate that by the preparation method, the reaction yield can be increased and the product quality can be improved.
Preparation method of pesticide intermediate 2-chloro-5-methyl pyridine
-
Paragraph 0019; 0036; 0041; 0042; 0050; 0055; 0056, (2019/02/08)
The invention discloses a preparation method of a pesticide intermediate 2-chloro-5-methyl pyridine. The preparation method comprises the following steps: adopting benzyl chloride, ammonia water and n-propanal as a starting material, and adopting a one-pot process to synthesize an intermediate (I); then using ion exchange resin as an acid-binding agent to carry out catalytic reaction, using acetylchloride as an acylation reagent to carry out acetylation, thereby obtaining an intermediate compound (II); and leading the intermediate compound (II), DMF (Dimethyl Formamide) and solid phosgene inan organic solvent to carry out cyclizing ring-closing reaction, thereby obtaining a target compound (I). The preparation method disclosed by the invention has the beneficial effects that the materials are cheap and easy to obtain, the reaction steps are fewer, the process operation is simple, the catalyst can be repeatedly utilized, the emission of three wastes is less, the process is pollution-free and environment-friendly, the product quality is good, the yield is high and the cost is low; the preparation method is very suitable for industrial production and has extremely-strong industrialapplication value.
Synthesis method of 2-chloro-5-chloromethylpyridine
-
Paragraph 0019-0029, (2018/04/03)
The invention discloses a synthesis method of 2-chloro-5-chloromethylpyridine. The synthesis method comprises the following main steps: 1, using 3-methylpyridine (I) as a main starting material and water as a reaction medium, performing a complete reaction on the 3-methylpyridine (I) and chlorine gas at 40-60 DEG C in the presence of a catalyst, and post-treating to obtain 2-chloro-5-methylpyridine (II) as a reaction raw material in the next step; 2, using the 2-chloro-5-methylpyridine (II) as the reaction raw material, in the presence or absence of a reaction medium, performing a complete reaction on the 2-chloro-5-methylpyridine (II) and the chlorine gas at 50-60 DEG C in the presence of the catalyst, and post-treating to obtain 2-chloro-5-chloromethylpyridine with the purity being higher than or equal to 99%. A reaction equation is as shown in the description. The method disclosed by the invention has the advantages of high reaction selectivity, stable product quality, simple production operation, increase in raw material utilization rate through combined use of the raw materials, reduction in production cost, and the like.
A 2 - chloro - 5 - methyl pyridine synthesis method
-
Paragraph 0020; 0022; 0024; 0026; 0027; 0028, (2018/03/26)
The present invention discloses a synthesis method of 2-chloro-5-methyl pyridine, and belongs to the technical field of pesticides. The method uses 2-amino-5-methylpyridine as the raw material. The method is as below: dissolving 2-amino-5-methylpyridine in concentrated hydrochloric acid; introducing excess of hydrogen chloride gas to generate saturation; dropwise adding nitric acid and thionyl chloride; after the reaction, neutralizing with alkali, layering, and separating an oil phase to obtain a product of 2-chloro-5-methyl pyridine. The method has the advantages of simple readily available raw materials, simple operation steps, rapid reaction, and simple separation of product.
A chloro pyridine and its derivatives synthetic method
-
Paragraph 0016; 0017, (2018/03/26)
The invention discloses a method for synthesizing chloropyridines and derivatives thereof and belongs to the field of fine chemical industry. According to the method, aminopyridine and derivatives thereof undergo a reaction to generate chloropyridines and derivatives thereof. The method is characterized in that phosphorus trichloride, phosphorus oxychloride or thionyl chloride and nitric acid are added into a solution of aminopyridine and the derivatives of aminopyridine, and chloropyridines and derivatives of chloropyridines can be obtained by stirring and reaction. The method has the advantages of being simple to operate, high in yield and less in three wastes.
2-chlorin-5-picoline preparation method
-
Paragraph 0019; 0021; 0022; 0023; 0025; 0028, (2018/04/03)
The invention discloses a 2-chlorin-5-picoline preparation method. According to the preparation method, 3-methylpyridine-N-oxide is utilized as a raw material, 2,4,6-triisopropyl-3-benzoyl chloride isutilized as a chlorinating agent, dichloromethane is utilized as a solvent, and chlorination reaction is performed under temperature of -20 to 50 DEG C to obtain 2-chlorin-5-picoline. According to the 2-chlorin-5-picoline preparation method disclosed by the invention, as the 2,4,6-triisopropyl-3-benzoyl chloride with a steric effect is utilized as the chlorinating agent, the defects that 2-chlorin-5-picoline prepared by a traditional method has poor selectivity and low yield are avoided, and yield of the 2-chlorin-5-picoline can be high as 95%; in addition, phosphorus oxychloride is preventedfrom being used, and the defect that phosphorus wastewater is difficult to treat is overcome.
