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以硝基甲烷和甲醛为原料,对合成溴硝醇的新方法进行了探讨,考察了反应温度,反应时间,反应后溶液的pH值以及重结晶使用的溶剂对产品收率的影响.最佳反应条件为:溴化反应温度为5℃,烷羟基化反应温度为25℃,反应时间为2h,反应完后溶液pH值调节在3之间,重结晶溶剂选择为V(乙酸乙酯):V(氯仿)=1:3的混合溶剂.
The new method of synthesizing bromotolon was studied by using nitromethane and formaldehyde as raw materials. The effects of reaction temperature, reaction time, the pH value of the solution after the reaction and the solvent used for recrystallization on the yield of the product were investigated. The reaction conditions were as follows: the temperature of bromination was 5 ℃, the temperature of alkylation was 25 ℃, the reaction time was 2h, and the pH value of the solution was adjusted to 3 after the reaction. The recrystallization solvent was selected as V (ethyl acetate) : V (chloroform) = 1: 3 mixed solvent.