广州化工
廣州化工
엄주화공
Guangzhou Chemical Industry
2015年
19期
41-43
,共3页
相转移催化法%四丁基溴化铵%(2-苯硫基乙基) 丙二酸二乙酯
相轉移催化法%四丁基溴化銨%(2-苯硫基乙基) 丙二痠二乙酯
상전이최화법%사정기추화안%(2-분류기을기) 병이산이을지
phase-transfer catalysis%tetrabutyl ammonium bromide%diethyl [2-(phenylthio) ethyl] malonate
采用相转移催化法,以丙二酸二乙酯和2-氯乙基苯硫醚为原料,四丁基溴化铵为催化剂,碱性条件下合成了(2-苯硫基乙基)丙二酸二乙酯。研究了四种碱对收率的影响,发现以叔丁醇钠作为碱时收率最高。同时,研究了各种反应条件对收率的影响,得到最佳条件为n(丙二酸二乙酯)：n(叔丁醇钠)：n(2-氯乙基苯硫醚)=1.3：1：1,100℃反应3 h。产物用1 H NMR和MS进行了表征。
採用相轉移催化法,以丙二痠二乙酯和2-氯乙基苯硫醚為原料,四丁基溴化銨為催化劑,堿性條件下閤成瞭(2-苯硫基乙基)丙二痠二乙酯。研究瞭四種堿對收率的影響,髮現以叔丁醇鈉作為堿時收率最高。同時,研究瞭各種反應條件對收率的影響,得到最佳條件為n(丙二痠二乙酯)：n(叔丁醇鈉)：n(2-氯乙基苯硫醚)=1.3：1：1,100℃反應3 h。產物用1 H NMR和MS進行瞭錶徵。
채용상전이최화법,이병이산이을지화2-록을기분류미위원료,사정기추화안위최화제,감성조건하합성료(2-분류기을기)병이산이을지。연구료사충감대수솔적영향,발현이숙정순납작위감시수솔최고。동시,연구료각충반응조건대수솔적영향,득도최가조건위n(병이산이을지)：n(숙정순납)：n(2-록을기분류미)=1.3：1：1,100℃반응3 h。산물용1 H NMR화MS진행료표정。
Diethyl [2-( phenylthio) ethyl] malonate was synthesized by the reaction of 2-chloroethyl phenyl sulfide and diethyl malonate in the presence of alkali, using tetrabutyl ammonium bromide as the catalysis under the phase transfer catalysis. The four kinds of alkali affected on the product yield were investigated, the reaction yield reached highest when using sodium tert-butoxide as alkali. The factoers influencd the reaction yield were studied, such as ratio of ratio of reagents, reaction temperature, and reaction time. The optimal reaction conditions were obtained when the molar ratios of diethyl malonate to sodium tert-butoxide to 2-chloroethyl phenyl sulfide at 1. 3:1:1, with the reaction temperature at 100℃, and the reaction time for 3 h, and the yield of product was 73%. The product was characterized by 1 H NMR and MS.
