摘要
采用对羟基苯乙酸(Ⅱ)和苯酞为原料,在甲醇钠的催化下,以n(Ⅱ)∶n(苯酞)∶n(甲醇钠)=1.0∶1.1∶2.2,于130℃反应7h制备4-(2-羧基苄氧基)苯乙酸(Ⅲ)。Ⅲ与乙酰氯经氯化、环合得6,11-二氢二苯骈[b,e]氧杂-11-酮-2-乙酸(Ⅰ),该步优化的反应条件为:n(Ⅲ)∶n(乙酰氯)=1∶1.25,反应温度为100℃,反应时间为6h。以Ⅱ计,总收率达48.16%,Ⅰ的结构经IR、1H NMR和MS确证。
4- （2-Carboxybenzyloxy）phenylacetic acid （ Ⅲ ） was synthesized from 4-Hydroxyphenyl acetic acid （ Ⅱ ） and phthalide in the presence of the catalyst sodium methoxide. The molar ratio of reactants （ Ⅱ ： phthalide ： sodium methoxide） was 1.0：1.1：2.2, the reaction time was 7 h and reaction temperature was 130℃. 6,11-Dihydro-11- oxodibenz [b ,e]oxepin-2-acetic acid （ Ⅰ ） was synthesized from Ⅲ and acetyl chloride through two-step reactions including chlorination and cyclization. The optimum reaction conditions were as follows： n （Ⅲ） ：n （acetyl chloride）=1 ： 1.25, reaction time 6 h and reaction temperature 100℃. The overall yield that was calculated from 11 was 48.16%. Structure of Ⅰ was characterized by IR, ^1H NMR and MS.
出处
《精细化工中间体》
CAS
2007年第2期39-41,共3页
Fine Chemical Intermediates
关键词
对羟基苯乙酸
苯酞
4-(2-羧基苄氧基)苯乙酸
环合
4-hydroxyphenyl acetic acid
phthalide
4- （2-carboxybenzyloxy）phenylacetic acid
cyclization
