广州化学
廣州化學
엄주화학
GUANGZHOU CHEMISTRY
2012年
2期
12-15
,共4页
朱玉梅%刘兰香%杨元法%罗孟飞
硃玉梅%劉蘭香%楊元法%囉孟飛
주옥매%류란향%양원법%라맹비
硼氢化钠%还原%二氟乙酸乙酯%二氟乙醇
硼氫化鈉%還原%二氟乙痠乙酯%二氟乙醇
붕경화납%환원%이불을산을지%이불을순
sodium borohydride%reduce%ethyl difluoroacetate%2,2-difluoroethanol
采用硼氢化钠(NaBH4)还原二氟乙酸乙酯(CF2HCOOCH2CH3)合成二氟乙醇(HCF2CH20H)。探讨NaBH4用量、溶剂、反应温度和反应时间等因素对反应的影响。实验结果表明:在投料比n(NaBH4)/n(CF2HCOOCH2CH3)=0.6,乙醇为溶剂,温度0℃反应条件下,二氟乙醇的收率可以达到98.1%。在极性溶剂中,随着反应温度的升高(5℃及以上),NaBI-14的分解加剧,低温对反应有利。
採用硼氫化鈉(NaBH4)還原二氟乙痠乙酯(CF2HCOOCH2CH3)閤成二氟乙醇(HCF2CH20H)。探討NaBH4用量、溶劑、反應溫度和反應時間等因素對反應的影響。實驗結果錶明:在投料比n(NaBH4)/n(CF2HCOOCH2CH3)=0.6,乙醇為溶劑,溫度0℃反應條件下,二氟乙醇的收率可以達到98.1%。在極性溶劑中,隨著反應溫度的升高(5℃及以上),NaBI-14的分解加劇,低溫對反應有利。
채용붕경화납(NaBH4)환원이불을산을지(CF2HCOOCH2CH3)합성이불을순(HCF2CH20H)。탐토NaBH4용량、용제、반응온도화반응시간등인소대반응적영향。실험결과표명:재투료비n(NaBH4)/n(CF2HCOOCH2CH3)=0.6,을순위용제,온도0℃반응조건하,이불을순적수솔가이체도98.1%。재겁성용제중,수착반응온도적승고(5℃급이상),NaBI-14적분해가극,저온대반응유리。
2,2-Difluoroethanol was obtained by reduction of ethyl difluoroacetate using sodium borohydride. Effects of reaction temperature, solvents, reaction time, sodium borohydride dosage, and so on were investigated. The results showed that n(NaBH4)/n(CF2HCOOCHECH3)=0.6, ethanol as solvent at 0℃, the yield of 2,2-difluoroethanol is 98.1% in the reaction. In polarity solvent, with reaction temperature rising (50C and above), the decomposition of the sodium borohydride intensifies, low temperature is favorite for the reaction.