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摘要为探究不同催化条件下Baeyer-Villiger反应的反应过程，优化旧式催化条件，避免使用有机过氧酸，减轻环境压力。为简化后期处理，提高原子经济性，使环境更加清洁，环保，故选用过氧化氢作为氧化剂，过渡金属氧化物作为催化剂，对2-庚基环戊酮进行氧化合成δ-十二内酯。通过改变催化剂的用量、反应的温度、反应时间、溶剂以及过氧化氢的质量来设计实验，并用气相色谱进行分析，测出转化率和产率。比较之后筛选出更加高效的，适用于工业化生产的Baeyer-Villiger反应催化条件。结果表明，0.55g 2-庚基环戊酮在0.06g MoO3，质量分数为50%的H2O2溶液催化条件下，40℃下反应12h，转化率可达到98.7%，产率最高可达到79.2%。25482
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关键词 Baeyer-Villiger反应 过氧化氢 δ-十二内酯 过渡金属
毕业论文设计说明书外文摘要
Title Synthesis of δ-dodecalactone
Abstract
As a green oxidation,hydrogen peroxide is environmentally-friendly and clearn ,which has been increasingly popular in organic synthesis.In this paper,we will introduce fragrance and flavours and design experiments according to these knowledge.what’s more,we also have a general description about the reasearch history and present state of the Baeyer-Villiger in detail. To learn more about the mechanism and to improve the conversion of the Beayer-Villiger oxidation reaction, avoiding environmental problems peracid brings, we will carry on experiments by using hydrogen peroxide as oxidations,transition metals as catalyst to oxidate 2-heptylcyclopentanone into δ-dodecalactone.The experiment indicate that the prime reaction conditions are 0.55g 2-heptylcyclopentanone and 0.4ml（2.5eq）hydrogen peroxide（50%） separately， 0.06 g WoO3 as catalyst reacting 12h at 40℃；the conversion can up to 98.7% and the yield rate is 79.2% . Some factors have great influence on the reaction,such as the polarity of solvent , the amount of catalyst, the amount and concentration of hydrogen peroxide,reaction temperature and time .All these factors have been designed .All results will show in this dissertation .（Shimadzu GC一2014C） gas chromatography will used as instrument to analyze the conversion of 2-heptylcyclopentanone and the yield ofδ-dodecalactone .And the foremost acid byproduct:5-oxours-dodecanoic was isolated and identified by 1H-NMR.
Keywords Baeyer-Villiger reaction 2-heptylcyclopentanone hydrogen peroxideWoO3
目 次
1引言 1
1.1 香精与香料 1
1.2 Baeyer-Villiger反应 2
2 实验部分 15
2.1 原料与产物的理化性质 15
2.2 实验试剂与实验设备 15
2.3 实验装置与实验过程 16
3 不同条件对Baeyer-Villiger反应的影响 18
3.1 不同催化剂催化的Baeyer-Villiger反应 18
3.2 不同质量MoO3催化的Baeyer-Villiger反应 19
3.3 不同温度下的Baeyer-Villiger反应 19
3.4 不同反应时间下的Baeyer-Villiger反应 20
3.5 不同溶剂下的Baeyer-Villiger反应 21
3.6 不同浓度H2O2下的Baeyer-Villiger反应 21
3.7 不同量的H2O2溶液下的Baeyer-Villiger反应 22
4 实验结果分析 23
4.1 理论产物分析 23
4.2 实际产物分析 23
4.3 催化Baeyer-Villiger反应的机理分析 24
5 总结 26