摘要
以2-硝基-3-氯苯甲酸为原料,由酰氯制备出酰胺后,经霍夫曼酰胺降解制得2-硝基-3-氯苯胺,研究了碱的用量、重排温度、脱羧温度和脱羧时间对降解反应的影响。当2-硝基-3-氯苯甲酰胺、氢氧化钾和溴的摩尔比为1：4：1,前后两次加入KOH的摩尔比为2.8：1.2,重排温度为40～45℃,脱羧温度为60～65℃,脱羧时间30 min时,所得产物的质量收率为30.0%,产物纯度大于98.0%。并对另一副产物的结构通过质谱和核磁进行了表征。
2-Nitro-3-chloroaniline was synthesized from 2-nitro-3-chloro benzoic acid via acylchloride formation,amidation and Hoffmann degradation.About Hoffmann degradation,the molar ratio of al- kaline,rearranging temperature,decarboxylating temperature and time were discussed.The results were as follows:molar ratio of 2-nitro-3-chlorobenzamide:potassium hydroxide:bromine=1:4: 1,molar ratio of pre-and post-addition of potassium hydroxide=2.8:1.2,rearranging temperature 40-45℃,decarboxylating temperature 60-65℃for 30 min,the yield is 30.0%,the purity of prod- uct could reach 98.0%.Besides these,the structure of one of the by-products was confirmed by MS and ~1H NMR.
出处
《精细石油化工》
CAS
CSCD
北大核心
2005年第4期8-10,共3页
Speciality Petrochemicals
