摘要
实验以邻甲酚为原料,以三光气保护酚羟基合成双(2-甲基苯酚)碳酸酯。研究了加料方式、反应物摩尔比、溶剂、催化剂、温度、碱的用量、母液回用等条件对收率的影响。实验结果表明,其最佳工艺条件为:当n(邻甲酚):n(三光气):n(氢氧化钠)=5.8:1.0:6.7,温度20℃,w(三乙胺)=2%。在此条件下,产物收率97.0%,纯度98.1%,反应母液套用后总收率达99.9%。
Di-o-tolyl carbonate was synthesized using o-cresol through protecting phenolic hydroxyl group by triphosgene with the yield of 97.0% and purity of 98.1%. The effects of feeding methods, molar ratio of raw materials, solvents, kinds of activators and dosage, temperature, dosage of sodium hydroxide on the reaction were discussed and the optimum conditions were found as follows： the molar ratio of o-cresol to triphosgene to sodium hydroxide of 5.8 ： 1.0 ： 6.7, reaction temperature about 20 ℃, triethylamine as the initiator with its dosage of 2% based on the triphosgene weight. The total yield of di-o-tolyl carbonate reached 99.9% when the mother solution was reutilized.
出处
《精细石油化工》
CAS
CSCD
北大核心
2010年第2期1-4,共4页
Speciality Petrochemicals
基金
江苏省精细化工重点实验室开放课题(BG2009015)
