摘要
以L-2-氨基丙酸为起始原料,经过重氮化、氧化、萃取、减压精馏步骤制得手性2-氯丙酸,并考察了原料配比、反应温度、酸浓度对反应的影响。最佳工艺条件为:n(L-丙氨酸):n(亚硝酸钠)为1:1.6,以(碳酸钠):n(L-丙氨酸)为1.2:1,盐酸浓度为25%,反应温度为5℃,反应时间为8h,在该条件下产品收率达72.0%,e.e.%值为97.6%~98.3%,比旋先度-14.6°。
A new process for the synthesis of L-2-chloropropanoic acid was proposed which involves four steps: diazotization, chlorination, extraction and rectifying to obtain the target L-2-chloropropanoic acid. The effects of raw materials amounts, reaction temperature, concentration of chlorhydrie acid on the reaction product yield were evaluated, and the optimum reaction conditions are: molar ratio of L-alanine to sodium nitrite 1: 1.6, molar ratio of sodium carbonate to L-alanine 1.2 : 1, concentration of hydrochloric acid 25%, temperature 5 ℃, reaction time 8 h. Under the optimum conditions, the yield of L-2- chloropropanoic acid could reach 72.0%. The ee value was between 97.6%-98. 3%, and the specific rotatory power -14.6.
出处
《化学世界》
CAS
CSCD
北大核心
2010年第1期40-42,共3页
Chemical World
关键词
L-2-氯丙酸
重氮化
氯化
L-2-chloropropanoic acid
diazotization
chlorination