摘要
利用超声振荡,以对硝基苯乙酮为原料,在原甲酸三乙酯和对甲苯磺酸的催化作用下和乙二醇醚化保护酮基,然后在氢氧化钠甲醇溶液的碱性条件下和苯乙腈环化加成,再用w(Pd)=5%的Pd-C催化加氢,最后在浓度为1mol/L的高氯酸的强酸作用下恢复酮基,合成出5 乙酰基 2 氨基二苯甲酮,用IR和1HNMR对其结构进行了表征。与非超声合成方法比较,反应时间由44h缩短到32h,目标产物总收率由39 5%提高到69 6%。
5Acetyl2aminobenzophenone is synthesized from pnitroacetophenone under the influence of ultrasonic.Firstly,pnitroacetophenone reacted with glycol in the presence of triethyl orthoformate and ptoluenesulfonic acid as catalyst to form ketal for protecting the keto group.Then cyclization was conducted with phenylacetonitrile in an alkaline solution of sodium hydroxide in methanol.In the third step catalytic hydrogenation was carried out using hydrogen gas in the existence of 5% palladium on carbon.Finally 5acetyl2aminobenzophenone was gained under the action of strong acid of 1 mol/L perchloric acid for restoration of the keto group.Structure of the target compound was identified by IR and 1HNMR.Compared with the conventional nonultrasonic synthetic method, the reaction time is shortened from 44 h to 32 h and the the yield of the object product is increased from 395% to 696%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2003年第10期638-640,共3页
Fine Chemicals
基金
国家973基金资助项目(51307)
