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采用一步法以二甲基二氯硅烷、四氢呋喃和金属镁粉为原料,在碘乙烷和单质碘催化下合成二-(4-羟基丁基)四甲基二硅氧烷。产物温合物减压过滤,以除去镁盐。滤液无需蒸馏提纯,而直接水解,干燥,减压蒸馏,收集71℃/1333Pa馏份。还探讨和优化合成条件:四氢呋喃与二甲基二氯硅烷之摩尔比应大于3.5;Grignard反应停止后应继续加热回流1小时;蒸馏时系统压力为1333Pa。
Di (4-hydroxybutyl) tetramethyldisiloxane was synthesized by one-step method using dimethyldichlorosilane, tetrahydrofuran and magnesium metal as raw materials under the catalysis of iodoethane and elemental iodine. Product warmer was filtered under reduced pressure to remove the magnesium salt. The filtrate without distillation purification, and direct hydrolysis, drying, vacuum distillation, collecting 71 ° C / 1333Pa fraction. Also to explore and optimize the synthesis conditions: tetrahydrofuran and dimethyldichlorosilane molar ratio should be greater than 3.5; Grignard reaction should continue to stop heating reflux for 1 hour; distillation system pressure 1333Pa.