相转移催化法合成2-氯-3-氯甲基-噻吩及噻康唑

相转移催化法合成2-氯-3-氯甲基-噻吩及噻康唑;相转移催化;氯氯甲基噻吩;氯甲基化;噻康唑

Synthesis of 2-Chloro-3-Chloromethyl-thiophene and Tioconazole via Phase Transfer Catalysis

The chloromethylation reaction of 2-chloro-thiophene via phase transfer catalysis was carried out to synthesize 2-chloro-3-chloromethyl-thiophene, where the catalyst was tetrabutylammonium bromide (TBAB ). The chloromethylation reagents used were paraformaldehyde and 37% concentrated hydrochloric acid. The structure of 2-chloro-3-chloromethyl-thiophene was confirmed by means of GC-MAS, IR and 1H NMR spectrometries. The yield was 77.6 %. The O-alkylation reactions between 1-(2,4-dichloro-phenyl)-2-( 1- imidazol)-ethanol and 2-chloro-3-chloromethyl-thiophene were performed in a two - phase system of organic solvent/solid NaOH under phase transfer catalytic condition. At the end, the tioconazole nitrate was formed by the addition of nitric acid. The structure of tioconazole was confirmed with IR and 1H NMR spectra. The yield of tioconazole was 53. 0% .