摘要
以硒催化在高压条件下还原2,5-二甲氧基-4-氯硝基苯制备2,5-二甲氧基-4-氯苯胺,通过条件实验确定了较好的反应条件:原料2,5-二甲氧基-4-氯硝基苯2.18 g(10 mmol)、Se 0.015 8 g、Na HCO_30.42 g(5mmol)、环己烷40 m L、H_2O 2m L;反应温度150℃;PCO 6.0 MPa;反应时间8 h。制备得2,5-二甲氧基-4-氯苯胺纯度可达98.38%,收率82.89%。通过正交试验,确定了各因素的影响强弱顺序为:反应时间>反应温度>CO压强>催化剂用量。
2,5-Dimethoxy- 4- chloroaniline was prepared from 4- chloro- 2,5- dimethoxy-nitrobenzene by high pressure reduction of CO/H2 O in cyclohexane solvent in the presence of catalyst selenium. The optimum condition was obtained by experiments： 4-chloro-2,5-dimethoxy-nitrobenzene 2. 18 g（ 10 mmol）,Se 0. 0158 g（ 0. 2 mmol）,Na HCO30. 42 g（ 5mmol）,cyclohexane 40 m L,H2 O 2m L,reaction temperature 150 ℃,PCO6. 0 MPa,reaction time 8 hours. The yield of 2,5-dimethoxy-4-chloroaniline was 82. 89%,the purity was 98. 38%. The effect order of different factors for the reduction was gotten by orthogonal experiments L9（ 34） ： reaction time 〉reaction temperature 〉 CO gas pressure 〉 the amount of selenium powder.
出处
《染料与染色》
CAS
2016年第3期24-26,5,共4页
Dyestuffs and Coloration
基金
辽宁省教育厅创新团队项目(LT2015012)的资金支持
