3-甲基-2-丁烯-1-醇的制备新工艺

研究了以溴代异戊烯水解工艺和精馏分离工艺为基础来制备3-甲基-2-丁烯-1-醇的新工艺。通过优化溶剂种类得到当水解溶剂为偶极类溶剂乙腈时,得到产物的选择性最高。并通过进一步优化实验操作条件,得到当溶剂加入量为v(乙腈):v(溴代异戊烯)=1:1,水解温度为70℃,碱用量为n(NaOH):n(溴代异戊烯)=1.2:1和反应时间为25min时,水解部分3-甲基-2-丁烯-1-醇的转化率最高可达63.35%。水解后的料液通过间歇精馏得到纯的3-甲基-2-丁烯-1-醇,最终的3-甲基-2-丁烯-1-醇总收率达到57.4%。

A new process on the preparation of 3-methyl-2-butene-1-ol

A new technology for the preparation of 3-methyl-2-butene-1-ol was investigated based on the hydrolysis of brominated isoamylene and distillation separation technology. By choosing a dipolar solvent, acetonitrile, for the hydrolysis the products showed the highest selectivity. And through further the optimization of experimental operating conditions, hydrolysis yield of 3-methyl-2-butene-1-ol reached 63.35% under the condition of the solvent amount v(acetonitrile):v(bromo-3-ene) = 1:1, hydrolysis temperature 70℃, base amount n(NaOH):n(bromo-3-ene) = 1.2:1 and reaction time 25 minutes. The pure 3-methyl-2-butene-1-ol was made of the feed liquid after hydrolysis by batch distillation operation, and the final total yield of 3-methyl-2-butene-1-ol reached 54%.