Paper
Study on synthesis of 2-chloromethyl-3-methyl-4-(2,2,2-trifluoroethyoxyl)-pyridine
Published 2011 · Xu Jun
Applied Chemical Industry
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Abstract
Using 2,3-dimethyl-byridine as the material,the process involved the following five steps:oxidation,nitration,substitution,acylation and chlorination,the total yield was 35.6%.The optimal synthetic condition of intermediate 2,3-dimethyl-4-(2,2,2-trifluoroethoxy)nitro-pyridine-N-oxide was:methyl iso-butylketone as the solvent and tetrabutyl ammonium bromide as the phase transfer catalyst,n(CF3CH2OH)∶n(K2CO3)∶n(2,3-dimethyl-4-nitro-pyridine-N-oxide)=4.5 ∶1.2 ∶1,reaction time 12 h,temperature 95 ℃,the yield of intermediate was 91.9%.The structure of intermediate was characterized by 1H NMR spectra,the target compound was 2,3-dimethyl-4-(2,2,2-trifluoroethoxy) nitro-pyridine-N-oxide.
The optimal synthetic conditions for 2,3-dimethyl-4-(2,2,2-trifluoroethoxy)nitro-pyridine-N-oxide were methyl iso-butylketone as solvent and tetrabutyl ammonium bromide as phase transfer catalyst, yielding 91
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