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中间体3-甲酰四氢噻喃的合成
Synthesis of 3-formyltetrahydrothiopyran
【摘要】 3-甲酰四氢噻喃是噻草酮的重要中间体,3-甲酰四氢噻喃的合成采用以丙烯醛和硫化氢为原料首先得到3-甲酰-5,6-二氢噻喃,然后3-甲酰-5,6-二氢噻喃在催化剂作用下氢化得到目标产物的合成路线.合成3-甲酰-5,6-二氢噻喃中,对丙烯醛投料方式、硫化氢投入量和催化剂选择进行了优化试验,提出了新的反应机理,使3-甲酰-5,6-二氢噻喃反应收率和质量分数分别达到93%和95%以上.制备3-甲酰四氢噻喃中,对催化剂进行了选择试验,发现用Raney-Ni作催化剂,目标产物的质量分数和收率达到92%和94%以上.
【Abstract】 3-Formyltetrahydrothiopyran is an intermediate of Cycloxydim.3-Formyltetrahydrothiopyran was prepared by hydrogenating a 3-formyl-5,6-dihydro-2H-thiopyran in the presence of a catalyst and 3-fromyl-5,6-dihydro-2H-thiopyran was prepared by reacting an acrolein with hydrogen sulfide.Under the optimal conditions of feeding method of arcolein,amount of hydrogen sulfide,and catalyst selection,the yield and purity of 3-formyl-5,6-dihydro-2H-thiopyran was more than 93% and 95%,respectively.A new reaction mechanism was proposed.Based on the optimized test of catalyst.3-Formyltetrahydrothiopyran had a yield above 94% and product content above 92% by using Raney-Ni as catalyst.
【Key words】 cycloxydim; 3-formyltetrahydrothiopyran; 3-formyl-5,6-dihydro-2H-thiopyran;
- 【文献出处】 浙江大学学报(理学版) ,Journal of Zhejiang University(Science Edition) , 编辑部邮箱 ,2007年06期
- 【分类号】TQ450
- 【被引频次】1
- 【下载频次】171