CAJ | 학술논문

以3,5-二羟基苯乙酮(4)为原料,经三步反应制得3,5-二乙酰氧基苯乙烯(1).在硫酸催化下化合物(4)与乙酸酐反应,得到3,5-二乙酰氧基苯乙酮(3),收率92%,对于化合物(3)进行了~1H NMR表征;化合物(3)经催化加氢,得到1-(1-羟基乙基)-3,5-二乙酰氧基苯(2),收率98%, 对于化合物(2)进行了~1H NMR表征;化合物(2)在固体酸催化下反应得到3,5-二乙酰氧基苯乙烯(1),制备化合物(1)的反应条件为: m[化合物(2)]∶m(固体酸)＝5∶1,110 ℃回流5 h,收率95%,纯度98%,对化合物(1)进行了IR,~1H NMR,MS表征,并对化合物(1)的1H NMR,MS表征结果进行了进一步分析.
이3,5-이간기분을동(4)위원료,경삼보반응제득3,5-이을선양기분을희(1).재류산최화하화합물(4)여을산항반응,득도3,5-이을선양기분을동(3),수솔92%,대우화합물(3)진행료~1H NMR표정;화합물(3)경최화가경,득도1-(1-간기을기)-3,5-이을선양기분(2),수솔98%, 대우화합물(2)진행료~1H NMR표정;화합물(2)재고체산최화하반응득도3,5-이을선양기분을희(1),제비화합물(1)적반응조건위: m[화합물(2)]∶m(고체산)＝5∶1,110 ℃회류5 h,수솔95%,순도98%,대화합물(1)진행료IR,~1H NMR,MS표정,병대화합물(1)적1H NMR,MS표정결과진행료진일보분석.
Diacetoxystyrene(1) was synthesized from 3,5-dihydroxyacetophenone(4) in a three-step process.3,5-Diacetoxyacetophenone(3) was synthesized from(4) and acetic anhydride with sulfuric acid as catalyst,the yield of (3) was 92%,(3) was identified by ~1H NMR;1-(1-hydroxyethyl)-3,5-diacetoxybenzene(2) was obtained by catalytic hydrogenation from (3),the yield of (2) was 98%,(2) was identified by ~1H NMR;(1) was obtained from (2) through a solid acid catalytic reaction,the reaction conditions were as follows: m (2) :m (solid acid)= 5: 1,reflux reaction time was 5 h at 110 ℃,the yield of (1) was 95% and the purity of (1) was 98%.(1) was identified by IR,~1H NMR,MS,the results of ~1H NMR of (1) and MS of (1) were resolved further.