摘要
以3-硝基-4-氯苯甲酸为原料,经水解反应得到产品,最佳水解条件为:氢氧化钠/3-硝基-4-氯苯甲酸摩尔比为4.5,碱液质量分数为15%,水解温度为95℃,反应时间为10 h。在最佳水解条件基础上,考察了碱液的循环利用,提高了氢氧化钠的利用率。总收率大于91%,纯度大于99%(HPLC),经FTIR、1H NMR、13C NMR和MS分析,证实产品为3-硝基-4-羟基苯甲酸。
3-Nitro-4-hydroxybenzoic acid was synthesized from 3-nitro-4-chlorobenzoic acid through hydro- lyzation in sodium hydroxide solution. Best result was obtained under conditions of reaction temperature of 95 ℃, molar ratio of sodium hydroxide to 3-nitro-4-chlorobenzoic acid of 4.5, mass concentration of sodium hydroxide of 15% ,reaction time of 10 h. Based on the optimized process, the recycle of sodium hydroxide was studied. High yield ( 〉 91% ) ,high purity ( 〉 99% HPLC was achieved. The structure of the title compound was confirmed by 1H NMR,13C NMR,FTIR and MS.
出处
《应用化工》
CAS
CSCD
2014年第2期332-334,共3页
Applied Chemical Industry