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以硝基苯甲醛为底物、高活性无水四甲基氟化铵(TMAFanh.)为氟化试剂,经氟代脱硝法一步合成了氟代苯甲醛,考察了反应温度、反应时间、溶剂和氟化剂等因素对氟代产物收率的影响。GC分析结果表明,在n(底物)∶n(TMAFanh.)=1∶1.4,底物为25mmol、DMF为10mL的条件下,低温即可实现对一些硝基苯甲醛类化合物的选择性亲核氟化,反应温度80~100℃,反应时间1~5h,氟代产物收率为19.4%~81.6%。原料易得、工艺简单、反应条件温和。
Using nitrobenzaldehyde as substrate and high activity anhydrous tetramethylammonium fluoride (TMAFanh.) As fluorinating agent, fluorobenzaldehyde was synthesized by fluorination and denitration method. The effects of reaction temperature, reaction time, solvent And fluorination agents and other factors on the yield of fluorinated products. The result of GC analysis showed that under the conditions of n (substrate): n (TMAFanh.) = 1: 1.4, substrate of 25 mmol and DMF of 10 mL, selective nitrobenzaldehyde The results showed that the yield of fluorinated products was 19.4% ~ 81.6% with the reaction temperature of 80 ~ 100 ℃ and the reaction time of 1 ~ 5 h. Easy to get raw materials, process is simple, mild reaction conditions.