Xi Qian
2015
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Journal
Journal of Wuhan Institute of Technology
Abstract
Aimed at complicated synthesis processes, low production rate of preparing 1,1-dihydroperfluorobutanol, heptafluorobutyric and methyl alcohol were applied as starting materials to prepare 1,1-dihydroperfluorobutanol. Via esterification with 4-toluene sulfonic acid as catalyst and reduction with sodium borohydride as reductant,1,1-dihydroperfluorobutanol was carried out. The results show that the yield of esterification reaction is 85% when the molar ratio of heptafluorobutyric to methyl alcohol is 2∶1, the mass ratio of catalyst to 4-toluene sulfonic acid is 0.6% and the refluxing time is 3 h; the optimal condition of reduction reaction is demonstrated when the reaction temperature is 30 ℃ and the molar ratio of reductant to ester is 0.8.The total yield is 77.35%, and the target product has characterized by nuclear magnetic resonance spectrum spectroscopy. This method is suitable for industry with mild conditions and low cost.