碳酸二甲酯作甲基化试剂合成间氯苯甲醚

用绿色化学原料碳酸二甲酯(DMC)代替硫酸二甲酯(DMS)等传统有毒试剂作为甲基化试剂,以间氯苯酚为原料,在固体碱与相转移催化剂(PTC)的作用下,合成了间氯苯甲醚。考察了PTC种类、物料配比、反应时间、反应温度和碱性催化剂用量对反应的影响,通过响应面实验设计,得到最佳反应条件:以四丁基溴化铵(TBAB)为PTC,K2CO3为碱性催化剂,n(间氯苯酚)∶n(DMC)∶n(TBAB)∶n(K2CO3)=1∶3.83∶1.07∶0.5,反应温度为98℃,反应时间为7 h,间氯苯甲醚的得率为98.3%,间氯苯酚的转化率为100%。

Synthesis of m-chloroanisole with Dimethyl Carbonate as Methylating Agent

m-chloroanisole was prepared from m-Chlorophenol in the presence of solid base and the phase transfer catalyst(PTC),using dimethyl carbonate(DMC) instead of dimethyl sulfate(DMS) as methylating reagent . The effect of solvent dosage, reactant mole ratio, reaction temperature and time on the conversion rate and yield of the product was studied. The optimum synthesis conditions were as follows through Response surface designs: Tetrabutyl ammonium bromide was used as PTC, Potassium carbonate was used as alkaline catalyst. n (m-Chlorophenol):n(DMC):n(Tetrabutyl ammonium bromide):n(Potassium carbonate)=1:3.83:1.07:0.5, reaction temperature 98oC, reaction time 7h. the yield of m-chloroanisole was 98.3% and the conversion rate of m-Chlorophenol was 100%.