5-Hydroxymethylthiazole is one of the most important medication and pesticide intermediates.5-Hydroxymethylthiazole was synthesized from 2-chloro-5-chloromethylthiazole through esterification with sodium acetate,reduc...5-Hydroxymethylthiazole is one of the most important medication and pesticide intermediates.5-Hydroxymethylthiazole was synthesized from 2-chloro-5-chloromethylthiazole through esterification with sodium acetate,reduction dechlorination on zinc/glacial acetic acid and hydrolysis with sodium hydroxide.For 0.05 mol 2-chloro-5-chloromethylthiazole,the results showed that the total yield of 5-Hydroxymethylthiazole was 68.3%(w(5-hydroxymethylthiazole)> 99%,GC peak area normalization method)under optimum conditions.The esterification was in 33% sodium acetate solution at 85 ℃ for 3 h;the reduction dechlorination on zinc/glacial acetic acid was the ratio of n(2-chloro-5-chloromethylthiazole)∶n(Zn)=1∶3 for 1 h;and the hydrolysis was in 25% sodium hydroxide solution at 70 ℃～75 ℃ for 2 h.The structure of 5-hydroxy-methylthiazole was confirmed by element analysis,IR,LC-MS,1H NMR and 13C NMR.展开更多
文摘5-Hydroxymethylthiazole is one of the most important medication and pesticide intermediates.5-Hydroxymethylthiazole was synthesized from 2-chloro-5-chloromethylthiazole through esterification with sodium acetate,reduction dechlorination on zinc/glacial acetic acid and hydrolysis with sodium hydroxide.For 0.05 mol 2-chloro-5-chloromethylthiazole,the results showed that the total yield of 5-Hydroxymethylthiazole was 68.3%(w(5-hydroxymethylthiazole)> 99%,GC peak area normalization method)under optimum conditions.The esterification was in 33% sodium acetate solution at 85 ℃ for 3 h;the reduction dechlorination on zinc/glacial acetic acid was the ratio of n(2-chloro-5-chloromethylthiazole)∶n(Zn)=1∶3 for 1 h;and the hydrolysis was in 25% sodium hydroxide solution at 70 ℃～75 ℃ for 2 h.The structure of 5-hydroxy-methylthiazole was confirmed by element analysis,IR,LC-MS,1H NMR and 13C NMR.
