摘要
以D-酒石酸与正庚醇为原料,在对甲苯磺酸催化下合成了手性拆分剂D-酒石酸正庚酯,通过正交实验确定优化反应条件为:D-酒石酸100 mmol,n(D-酒石酸)∶n(正庚醇)=1.0∶2.6,对甲苯磺酸0.5 g,甲苯50mL,回流反应约1 h,酯化率99%,收率在93%以上。其结构经IR确证。
A chiral resolving reagent, n-heptyl D-tartrate, was synthsized from D-tartaric acid and n-heptanol using p-toluene sulfonic acid as a catalyst by refluxing for 1 h. The effect of molar ratio of reaetant, amount of solvent and catalyst and stir speed on the yield were discussed by orthogonal test. The optimum reaction conditions were as fillows: the molar ratio of D-tartaric acid to n-heptanol was 1.0 : 2.6, the amount of p-toluene sulfonic acid was 0.5 g, and toluene was 50 mL. The yield was about 93% and the esterification rate was over 99% under the optimum reaction conditions. The structure was confirmed by IR.
出处
《合成化学》
CAS
CSCD
2006年第1期82-83,105,共3页
Chinese Journal of Synthetic Chemistry
基金
国家自然科学基资助项目(20376085)
湖南省自然科学基金资助项目(03JJY3020)
关键词
手性
拆分
酒石酸
正庚醇
酯化
chiral
resolve
tartaric acid
heptanol
esterification
作者简介
陈国斌(1944-),男,教授,主要从事应用化学与分析方面的研究。Tel.0730-8847076,E-mail:cgb076@126.com