期刊论文

Luo, Y.-M.(luoyiming68@hotmail.com)

中文

中南大学学报(自然科学版)

1672-7207

2006

37

3

521-526

10.3969/j.issn.1672-7207.2006.03.020

20436010:国家高技术研究发展计划（863计划）

本校为其他机构

采用GC-MS方法分析反应产物，对氯酸钠氧化β-紫罗兰酮的反应工艺进行研究，并探讨温度、时间、反应物配比和溶液的pH值对反应的影响。反应产物的结构采用红外光谱、质谱、氢核磁共振谱和元素分析等手段表征。研究结果表明：氯酸钠氧化β-紫罗兰酮的反应主要生成4-氧代-β-紫罗兰酮和5，6-环氧-β-紫罗兰酮，经重结晶和硅胶柱层析分离，纯度高于98％；4-氧代-β-紫罗兰酮的有利合成条件是反应温度为45℃，反应时间为24h，溶液的pH值为1～3，反应物配比n（β-ionone）：n（NaClO3）：n（NaI）为20：100：3，最佳收率为53．5％；5，6-环氧-β-紫罗兰酮有利的合成条件是反应温度为40℃，反应时间为...

The procedure of oxidation of β-ionone by sodium chlorate was studied using gas chro-matography-mass spectrometry to analyze the reaction products. And their structures were characterized by IR, MS, 1HNMR and EA. The effect of reaction temperature, reaction time, molar ratio of reactants and pH value of solution were investigated. Results show that 4-oxo-β-ionone is the major product with yield of 53.5% under the conditions as follows: reaction temperature 45 °C, reaction time 24 h, the molar ratio of n(β-ionone) : n(NaClO3) : n(Nal) 20 = 100 : 3, and pH value of solution in...