13600-43-6Relevant articles and documents
Preparation process 4 - trifluoromethyl nicotinic acid
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Paragraph 0021; 0024-0025; 0027; 0030-0031; 0033; 0036-0037, (2021/10/11)
The invention discloses a preparation process of 4 -trifluoromethyl nicotinic acid and vinyl ether. Trifluoracetyl chloride and catalyst were added to the reactor and stirred. Acylation to obtain 4 - ethoxy -1, 1, 1 -trifluoro -3 - alkene -2 - ketone, reacting 4 - with a catalyst and an oxidizing agent to -1 ethoxy 1, 1 -3 -trifluoro -2 -butenone, 25 - 90 °C g 30 - 60min of 1-trifluoroethyl 1-butenecone, adding 1 - equivalents of alkali lye, and then acidifying to obtain -4 - 2-trifluoromethylnicotiniconicotinic acid, followed by acidification with -3 - 4 -chloro 1 - 5-4 - trifluoromethyl POCl3 picolinic 6 - acid -4 . The preparation method of 4 -trifluoromethyl nicotinic acid is optimized. Only the reaction temperature is controlled, the intermediate product can be used for subsequent reaction steps, the reaction requirements in the step process are reduced, the requirement for equipment is low, and industrialization can be conveniently realized.
Method for preparing 4-(trifluoromethyl)nicotinic acid
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Paragraph 0028-0033, (2019/03/29)
The invention discloses a method for preparing 4-(trifluoromethyl)nicotinic acid, and belongs to the technical field of methods for preparing chemical pharmaceutical intermediates. The method comprises steps of using trifluoroacetyl chloride, vinyl ethyl ether and 3-aminoacrylonitrile as raw materials to prepare the 4-(trifluoromethyl)nicotinic acid through acylation, cyclization and hydrolysis reactions. The method provided by the invention is relatively cheap and easily available in adopted raw material, simple and convenient to operate, easy in separation and purification of products in each step, high in yield, and more suitable for industrial production.
4-Position-Selective C-H Perfluoroalkylation and Perfluoroarylation of Six-Membered Heteroaromatic Compounds
Nagase, Masahiro,Kuninobu, Yoichiro,Kanai, Motomu
, p. 6103 - 6106 (2016/06/09)
The first 4-position-selective C-H perfluoroalkylation and perfluoroarylation of six-membered heteroaromatic compounds were achieved using nucleophilic perfluoroalkylation and perfluoroarylation reagents. The regioselectivity was controlled by electrophilically activating the heteroaromatic rings, while sterically hindering the 2-position, with a sterically bulky borane Lewis acid. The reaction proceeded in good yield, even in gram scale, and by a sequential reaction without isolating the intermediates. This reaction could be applied to late-stage trifluoromethylation of a bioactive compound.
