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作 者:陈云华[1] 叶海伟[1] 童华光 周丽萍[1] 王恩建 CHEN Yun-hua;YE Hai-wei;TONG Hua-guang;ZHOU Li-ping;WANG En-jian(Chemical Pharmaceutical Research Institute,Taizhou Vocational&Technical College,Taizhou 318000,China;Taizhou Daozhi Tech Co.,Ltd.,Taizhou 318000,China)
机构地区:[1]台州职业技术学院化学制药研究所,浙江台州318000 [2]台州道致科技股份有限公司,浙江台州318000
出 处:《精细化工中间体》2023年第2期23-26,共4页Fine Chemical Intermediates
基 金:台州市科技计划项目(22gya10);浙江省教育厅一般科研项目(Y202147360)。
摘 要:3-(三甲基硅基)丙炔酰氯是合成防治小麦全蚀病杀菌剂硅噻菌胺的重要中间体,以丙炔醇■为起始原料,经硅烷化后与格氏试剂发生三甲基硅基交换得3-(三甲基硅基)丙炔醇■经2,2,6,6-四甲基哌啶氧化物(TEMPO)催化氧化得3-(三甲基硅基)丙炔醛■经氯代得3-(三甲基硅基)丙炔酰氯■,纯度98%(GC),总收率78%。产物经~1H NMR、^(13)C NMR和MS结构表征确证。该合成方法反应条件温和、收率较高、经济性好、便于生产,具有工业化前景。3-(Trimethylsilyl)propynoyl chloride is an important intermediate in the synthesis of silthiopham,a fungicide used to control wheat take-all diseases.Propargyl alcohol■ was used as the raw material that first went through a silanization reaction,which was then followed by a exchange reaction with grignard reagent to prepare■The target compound ■in purity of 98%(GC) and overall yield of 78% was synthesized by oxidation reaction and chlorination reaction form■,and the structure of the product was characterized by~1H NMR,^(13)C NMR and MS spectra.The advantages of the present procedure include mild reaction condition,satisfactory yields and easy operation.Therefore it may be promising for industrial application.
关 键 词:3-(三甲基硅基)丙炔酰氯 硅噻菌胺 优化 合成
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