摘要
以二乙二醇单甲醚(C5H12O3)和氢氧化钠为原料,n(NaOH):n(C5H12O3)=1.5:1.0(mol/mol),减压条件下,先合成二乙二醇单甲醚醇钠盐,然后通入CH3Cl与二乙二醇单甲醚钠盐进行Williamson反应合成二甘醇二甲醚。较为系统研究了反应温度、反应时间及n(NaOH)/n(C5H12O3)的摩尔配比等因素对反应的影响。用FTIR和NMR分析测试手段表征了产物结构。实验结果表明该反应的较优工艺条件为:n(NaOH)/n(C5H12O3)/n(CH3Cl)=1.5:1.0:1.4,反应温度为90~100℃,CH3Cl通入时间为5.0h,二甘醇二甲醚的收率可这95.0%以上。
Diethylene glycol mono-methyl ether monosodium salt was prepared from diethylene glycol mono-methyl ether (C5H12O3 ) and sodium hydroxide under vacuum pressure condition and n(NaOH)/n(C5H12O3 ) = 1.5:1.0. Then diethylene glycol dimethyl ether (DMDE) was synthesized through Williamson reaction from CH3Cl and CH3OCH2CH2OCH2CH2ONa. The influencing factors, such as reaction temperature, reacticn time and n(CH3Cl)/n(C5H12O3 ), ere were investigated. The product was identified by FT IR and NMR. The results indicated that the suitable Williamson reaetion conditions were as follows: n ( NaOH ) / n ( C5H12O3 ) / n( CH3Cl) = 1.5 : 1.0 : 1.4 ; reaction temperature, 90 - 100℃; reaetion time, 5.0 h. The yield of DMDE could reach over 95.0%.
出处
《化学世界》
CAS
CSCD
北大核心
2006年第7期417-419,共3页
Chemical World
关键词
二甘醇单甲醚钠盐
二甘醇二甲
Williamson反应
合成
diethylene glycol mono-methyl ether mono-sodium salt
diethylene glycol dimethyl ether
Williamson reaction
synthesis