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从5-氯-1-茚酮出发,用碳酸二甲酯(DMC)代替传统的有毒有害试剂作为甲氧羰基化试剂兼作溶剂,在NaH作用下,一步合成了5-氯-2-甲氧羰基-1-茚酮。考察了原料摩尔比、反应温度、滴加时间对产品质量和收率的影响。确定了最佳反应条件:n(5-氯-1-茚酮)∶n(NaH)=1∶3,反应温度90℃,滴加时间30 m in,收率达到86.09%。所得产品的结构经FTIR、1HNMR1、3CNMR和MS进行了表征。已在浙江宏元医药化工有限公司实施中试开发。
Starting from 5-chloro-1-indanone, dimethyl carbonate (DMC) was used as a methoxycarbonylation reagent in place of traditional toxic and hazardous reagents as a solvent. Under the action of NaH, 5-chloro-2- Carbonyl-1-indanone. The effects of molar ratio of raw materials, reaction temperature and dropping time on product quality and yield were investigated. The optimal reaction conditions were as follows: n (5-chloro-1-indanone): n (NaH) = 1: 3, reaction temperature 90 ℃, dropping time 30 min, yield 86.09%. The structure of the obtained product was characterized by FTIR, 1HNMR1, 3CNMR and MS. In Zhejiang Hongyuan Pharmaceutical Chemical Co., Ltd. pilot development.