化合物2,2-二甲基环戊酮合成工艺研究
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摘要
以己二酸二甲酯为原料,在甲醇钠作用下关环,然后经过硫酸二甲酯甲基化作用,再经过脱脂反应得到中间体2-甲基环戊酮,最后在硫酸二甲酯甲基化作用下得到2,2-二甲基环戊酮。在2,2-二甲基环戊酮合成过程中考察了溶剂种类、反应温度、甲基化试剂种类及用量对甲基化作用的影响,得到以甲苯为溶剂、反应温度为35℃、硫酸二甲酯为甲基化试剂、2-甲基环戊酮与硫酸二甲酯比例为1∶1的最优甲基化工艺条件。
As raw material,dimethyl adipate was closed loop under sodium methylate, then methylation was happened by dimethyl sulfate, following the intermediate 2-methylcyclopentanone was obtain after degreasing reaction. Finally, 2,2-dimethylcyclopentanone was obtained by methylation of dimethyl sulfate. In the synthesis of 2,2-dimethylc-yclopentanone, the effects of solvent type, reaction temperature, type and dosage of methylation reagent on methylation were investigated. The optimum methylation conditions were obtained with toluene as solvent, reaction temperature 35°C, dimethyl sulfate as methylation reagent, and the ratio of 2-methylcyclopentanone to dimethyl sulfate was 1∶1.
As raw material,dimethyl adipate was closed loop under sodium methylate, then methylation was happened by dimethyl sulfate, following the intermediate 2-methylcyclopentanone was obtain after degreasing reaction. Finally, 2,2-dimethylcyclopentanone was obtained by methylation of dimethyl sulfate. In the synthesis of 2,2-dimethylc-yclopentanone, the effects of solvent type, reaction temperature, type and dosage of methylation reagent on methylation were investigated. The optimum methylation conditions were obtained with toluene as solvent, reaction temperature 35°C, dimethyl sulfate as methylation reagent, and the ratio of 2-methylcyclopentanone to dimethyl sulfate was 1∶1.
引文
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[7]Banitt,Elden H.Cyclopentanone derivatives[P].US:4497954,1985-2-5.
[8]Wong,George S K.A process for the preparation of 2,2-dimethyl-5(4-chlorobenzyl)cyclopentanone and an intermediate useful therefore[P].EP:01953167.2,2002-01-31.
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