770-11-6Relevant articles and documents
A 4 - ( chlorine two fluorine methoxy ) method for preparing aniline
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Paragraph 0016; 0026; 0027; 0028; 0029, (2018/02/04)
The invention relates to a preparation method for 4-(chlorodifluoromethoxy)aniline. The method includes: taking trichloromethoxybenzene as the raw material, employing hydrogen fluoride to conduct selective fluorination to obtain chlorodifluoromethoxybenze
Selective fluorination of substituted trichloromethyl benzenes by HF in liquid phase: Preparation of fluorinated building blocks
Piou, Alexandre,Celerier, Stephane,Brunet, Sylvette
experimental part, p. 1241 - 1246 (2011/01/12)
The selective fluorination by successive Cl/F exchanges of α,α,α-trichlorotoluene, substituted or not by a chlorine atom, was studied in the presence of HF as the fluorinating agent. The influence of the presence of a catalyst or a basic solvent (such as dioxane, pyridine, tributylphosphate) in order to control the fluorination was also investigated. In mild conditions (50 °C and after 1 h of reaction), HF in excess was required in order to obtained the trifluoromethylation by Cl/F exchanges. The presence of SbCl5 in small amount activated the Cl/F exchanges and only a stoichiometric amount of HF was required whatever the chlorinated molecules. Selective mono and difluorination could be obtained by using basic solvents.
Synthesis conditions and activity of various Lewis acids for the fluorination of trichloromethoxy-benzene by HF in liquid phase
Salomé,Mauger,Brunet,Schanen
, p. 1947 - 1950 (2007/10/03)
The experimental conditions (temperature, reaction time, amount of hydrogen fluoride (HF)) for the comparison of the performances of various Lewis acids in the liquid phase fluorination by HF of the trichloromethoxy-benzene were determined by using SbCl5 as the reference catalyst. After 1h reaction at 50°C, C6H5OCCl3 was totally converted into C6H5OCF3 requiring only 2mol% of SbCl5 and a stoichiometric amount of HF. The most efficient catalysts were found to be chlorinated Lewis acids in which the metal is at the state of oxidation +V (SbCl5, MoCl5, TaCl5 and NbCl5). The appropriate catalyst has to be able to form a nucleophilic complex with HF, which constitutes the actual fluorinating agent and is more efficient than HF alone.