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以3-甲氧基苯甲醛为原料,经亨利反应、还原硝基和双键、氨基保护、傅-克酰基化、脱甲基、环合、羰基还原等反应,合成目的产物6-2-氨丙基-2,3-二氢苯并呋喃。并对硝基和双键的还原反应、傅-克酰基化和脱甲基反应的工艺条件进行了优化,得出较佳工艺条件:(1)化合物Ⅱ的还原反应:反应温度40℃,氢气压力4.0 MPa,Raney-Ni用量为化合物Ⅱ质量的8%,产物收率为78.6%;(2)合成化合物Ⅵ的反应:反应温度45℃,n(氯乙酰氯)/n(化合物Ⅳ)=1.4,反应时间6 h,产物收率为68.8%。
Using 3-methoxybenzaldehyde as raw material, the target product was synthesized by the reaction of Henry reaction, reduction of nitro and double bonds, protection of amino group, Friedel-Crafts acylation, demethylation, cyclization and carbonyl reduction. Aminopropyl-2,3-dihydrobenzofuran. The reduction conditions of nitro group and double bond, Friedel-Crafts acylation and demethylation were optimized. The optimum conditions were obtained as follows: (1) The reduction of compound Ⅱ: the reaction temperature was 40 ℃, the hydrogen The reaction pressure is 4.0 MPa, the amount of Raney-Ni is 8% of the mass of compound II, and the yield of product is 78.6%. (2) The reaction of compound VI: reaction temperature 45 ℃, 1.4, reaction time 6 h, product yield 68.8%.