摘要
以6-氯烟酸(Ⅰ)为原料,在N-甲基吗啉的催化下,与氯甲酸乙酯反应成酸酐活化羧基,再与干肼缩合,合成6-氯烟酸酰肼,考察了物料配比、反应温度、反应时间对收率的影响。结果表明,合成6-氯烟酸酰肼的最佳工艺条件为:n(Ⅰ)∶n(氯甲酸乙酯)∶n(N-甲基吗啉)∶n(肼)=1∶1.2∶1.5∶5,反应温度为-5℃,两步反应的反应时间均为2 h,收率可达83%。
6-Chloro-nicotinic acid hydrazide was prepared from 6-chloro-nicotinic acid in the catalysis of N-methyl-morpholine by two steps including the activation reaction of carboxyl group and the substitution reaction with anhydrous hydrazine. Effect of the ratio of reagents, the reaction temperature and reaction time on yield were invest/gated. The result showed that the optimized conditions were obtained： n（ I ）： n（6-chloro-nicotinie acid） ： n （N-methyl-morpholine） ： n （hydrazine） = 1： 1.2： 1.5：5, temperature -5 ℃ ,the reaction time of two steps 2 h,the yield was up to 83%.
出处
《应用化工》
CAS
CSCD
2013年第12期2255-2257,共3页
Applied Chemical Industry
关键词
6-氯烟酸酰肼
6-氯烟酸
合成工艺
6-chloro-nicotinic acid hydrazide
6-chloro-nicotinic acid
synthesis technology
