摘要
以Se/CO/H2O体系还原制备CLT酸,通过改变反应溶剂实现了由高压反应到常压反应的转化。在一系列条件实验的基础上确定了相对较优的反应条件:原料2 g(3.35 mmol);Se 0.0158 g(0.2 mmol);DBU 0.06 g;H2O 2 m L;N,N-二甲基苯胺20 m L;反应温度80℃;反应时间10 h,CLT酸收率97.74%,纯度89.60%。
CLT acid was prepared by atmospheric pressure reduction of CO/H20 in the presence of catalyst selenium. High pressure reaction is transformed into the atmospheric reaction by changing the reaction solvent. The optimum condition was obtained by experi- ments: ingredients 2 g (3.35 mmol) ; Se 0. 0158 g (0. 2 mmol) ; DBU 0.06 g; H20 2 mL; N, N-dimethyl aniline 20 mL; reaction temperature 180 ℃ ; reaction time 10 hours, CLT acid yield was 97.74%, the purity of 89. 60%.
出处
《染料与染色》
CAS
2015年第2期26-28,共3页
Dyestuffs and Coloration
基金
辽宁省教育厅自然基金(L2012002)
创新团队项目(LT2012001)
沈阳市重点实验室项目(F13-289-1-00)的资金