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中间体3-甲酰四氢噻喃的合成

Synthesis of 3-formyltetrahydrothiopyran

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【作者】 谭成侠孙娜波翁建全沈德隆曹耀艳

【Author】 TAN Cheng-xia,SUN Na-bo,WENG Jian-quan,SHEN De-long,CAO Yao-yan(College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou 310032,China)

【机构】 浙江工业大学化学工程与材料学院浙江工业大学化学工程与材料学院 浙江杭州310032浙江杭州310032

【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.

【基金】 浙江省科技厅资助项目(200101010)
  • 【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
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