摘要
以2-叔丁基苯酚、镁和多聚甲醛为原料,甲醇为溶剂,经甲酰化反应合成了3-叔丁基水杨醛,再经溴化反应合成了5-溴-3-叔丁基水杨醛。考察了溶剂、反应温度、物料比等对产品收率的影响。5-溴-3-叔丁基水杨醛合成的较优条件为:n(3-叔丁基水杨醛)∶n(液溴)=1∶1.1,反应溶剂为乙醇,反应温度60℃,反应时间8h,产品经1 H-NMR表征确认。
3-tert-butyl-2-hydroxybenzaldehyde was synthesized from 2-(tert-butyl) phenol, magnesium scraps and paraformaldehyde in methanol by formylatioru Then 5-bromo-3-tert-butyl-2-hydroxy-benzaldehyde was synthe- sized from bromine and 3-tert-butyl-2-hydroxybenzaldehyde. The solvent, reaction temperature, material ratio were investigated. The optimal conditions of 5-bromo-3-tert-butyl-2-hydroxy-benzaldehyde were obtained as follows: sol- vent of ethylalcohol, n(3-tert-butyl-2-hydroxybenzaldehyde) : n (Br2) :1 : 1.1, temperature of 60 ℃,reaction time of 8 h, 1H-NMR characterization was employed to confirm the target compounds.
基金
安徽大学青年科学研究基金(2009QN010A)
关键词
3-叔丁基水杨醛5-溴-3-叔丁基水杨醛合成优化
3-tert-butyl-2-hydroxy-benzaldehyde, 5-bromo-3-tert-butyl-2-hydroxy-benzaldehyde, synthesis, optimization