3-氨基-1,2-丙二醇的合成与表征

以3-氯-1,2-丙二醇和氨水为原料合成了3-氨基-1,2-丙二醇,并引入活性炭脱色和氨回收工艺,及分子蒸馏技术。考察了原料摩尔比、反应温度和反应时间等因素对产物收率的影响,当n(氨):n(3-氯-1,2-丙二醇)=15:1,反应温度为50℃,反应时间为4 h,采用分子蒸馏分离产物时,3-氨基-1,2-丙二醇的收率为90%,产物纯度为99.6%。采用元素分析、IR、~1H NMR和~(13)C NMR对产物进行了表征。

SYNTHESIS AND CHARACTERIZATION OF 3-AMINO-1,2-PROPANEDIOL

3-Amino-1,2-propanediol was prepared from 3-chloro-l,2-propanediol and ammonia.The process of activated charcoal decoloration,ammonia recovery and molecular distillation were introduced. The effects on the yield were investigated,such as the molar ratio of ammonia and 3-chloro-1, 2-propanediol,reaction temperature and reaction time.The yield of product was 90%and the purity was 99.6%under optimized conditions that n(ammonia):n(3-chloro-1,2-propanediol) = 15:1,reaction temperature was 50℃,reaction time was 4 h,and the separation process was molecular distillation. The structure of target compound was characterized by elemental analysis,IR,~1H NMR and ~(13)C NMR.