69045-84-7Relevant articles and documents
Preparation method of 2, 3-dichloro-5-trifluoromethylpyridine
-
Paragraph 0025-0038, (2021/08/14)
The invention discloses a preparation method of 2, 3-dichloro-5-trifluoromethylpyridine, and belongs to the technical field of organic synthesis. The comprises the following steps: (1) adding 2, 3-dichloro-5-trichloromethylpyridine into an organic solvent under the condition of 20 to 50 DEG C, so as to obtain an organic solution of 2-chloro-5-trichloromethylpyridine; (2) adding fluorinated quaternary ammonium salt and 1, 2-dicyanotetrafluorobenzene into the organic solution of the 2, 3-dichloro-5-trichloromethylpyridine obtained in the step (1), and uniformly mixing to obtain a reaction system; 3) controlling the temperature of the reaction system to be 30-60 DEG C, and reacting to obtain 2, 3-dichloro-5-trifluoromethylpyridine; and 4) filtering the reaction liquid, and carrying out reduced pressure distillation on the obtained filtrate to obtain the 2, 3-dichloro-5-trifluoromethylpyridine. The method can be completed in one step, cheap fluorinated quaternary ammonium salt is selected as a fluorination reagent, and operation is easy; the raw materials are cheap and easily available, the reaction temperature is low, the reaction time is short, and conditions such as high-temperature, high-pressure and dangerous hydrogen fluoride raw materials are avoided; and the yield of the obtained product is 70-90%, and the gas chromatography detection purity is greater than 99.0%.
Preparation method of 2,3-dichloro-5-trifluoromethylpyridine
-
Paragraph 0050; 0073-0079, (2021/10/27)
The invention provides a preparation method of 2,3-dichloro-5-trifluoromethylpyridine. The method comprises the following steps: carrying out condensation and acidification on 1, 1, 1-trifluoroacetone and nitromethane under the action of alkali to obtain 1-nitro-2-trifluoromethyl propylene; the method comprises the following steps: condensing 1-nitro-2-trifluoromethyl propylene and oxalic acid diester under the action of alkali, and carrying out reduction-cyclization reaction and acidification reaction on the obtained reaction liquid in the presence of a catalyst without separation to obtain a product 2, 3-dihydroxy-5-trifluoromethylpyridine; and then subjecting the 2,3-dihydroxy-5-trifluoromethylpyridine and a chlorination reagent to a chlorination reaction to obtain the 2,3-dichloro-5-trifluoromethylpyridine. The raw materials used in the invention are cheap and easily available, and the reaction selectivity of each step is high. The process does not need special equipment to carry out high-temperature chlorination and high-temperature fluorination reactions and is easy to operate, the target product is high in yield and purity, and the process is suitable for industrial production.
Synthetic method of 2,3-dichloro-5-trifluoromethylpyridine
-
Paragraph 0023; 0024; 0025; 0025; 0026-0030, (2017/04/29)
The invention discloses a synthetic method of 2,3-dichloro-5-trifluoromethylpyridine. The method comprises the following steps that 1,2,3-dichloro-5-trichloromethylpyridine and hydrogen fluoride are subjected to a halogen exchange reaction at the temperature of 140-200 DEG C under the action of a catalyst; 2, the product obtained after the halogen exchange reaction is heated at the pressure of 0.15-1.0 MPa for a pressurizing conversion reaction, and 2,3-dichloro-5-trifluoromethylpyridine is obtained. According to the method, 1, 2,3-dichloro-5-trichloromethylpyridine and hydrogen fluoride are used for the reaction; the method is characterized in that under catalysis of the catalyst, trichloromethylpyridine reacts with hydrogen fluoride, the reaction is carried out at normal pressure at first, then the conversion reaction is carried out under certain pressure and temperature, and therefore the defect that in a traditional process, it is dangerous because a reaction is carried out at high temperature and high pressure is overcome. According to the process, reaction conditions are mild, dangerousness is low, a small quantity of waste gas, waste water and waste solids are produced, and separation is easy.