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为降低成本,在无溶剂的条件下,以氢氧化钠固体为催化剂,环己醇和硝基甲烷直接加成,合成了1-硝甲基环己醇。对产品做了红外检测、折光率测定以及气相色谱分析;探讨了反应条件对产品产率的影响,找出了较佳的工艺合成条件。结果表明,合成较佳工艺条件为:反应时间为10 h;反应温度15℃;硝基甲烷和环己酮的投料摩尔比为1.2:1;碱催化剂与硝基甲烷的摩尔比为1:4;制得硝甲基环己醇产率为59.45%。
In order to reduce the cost, 1-nitromethylcyclohexanol was synthesized by the direct addition of cyclohexanol and nitromethane under solvent-free conditions with sodium hydroxide solid as catalyst. The infrared detection, refractive index measurement and gas chromatography analysis were done on the products. The effects of reaction conditions on the yield of the products were discussed, and the better synthesis conditions were found out. The results showed that the best synthesis conditions were as follows: the reaction time was 10 h; the reaction temperature was 15 ℃; the molar ratio of nitromethane to cyclohexanone was 1.2: 1; the molar ratio of base catalyst to nitromethane was 1: 4 The yield of nitromethylcyclohexanol was 59.45%.