摘 要:本篇论文的研究目标是:用硼氢化钠作为催化剂还原3,7-二甲基-3-乙酰硫基-6-辛烯醛,最终对产物进行分离提纯及结构鉴定,确定最终产物。用硼氢化钠作为催化剂还原3,7-二甲基-3-乙酰硫基-6-辛烯醛的反应是一个升温反应。首先搭建一套蒸馏装置,在三口烧品中放入已经称量好的3,7-二甲基-3-乙酰巯基-6-辛烯醛和硼氢化钠,在三口烧瓶下放置一个冰水浴装置,开启冷凝水并缓慢搅拌。持续搅拌2.5-3小时左右,加10毫升冰水猝灭反应,用15%稀盐酸调节pH到溶液呈中性。搭建一套分液装置,将分液漏斗架在具有铁圈的铁架台上,并且用乙酸乙酯萃取反应液,有机层用饱和氯化钠洗2-3次,分液,分液后用无水硫酸钠干燥。放置过夜,第二天使用旋蒸仪将粗产物旋蒸提纯。将产物进行点板,并使用图谱分析检验产物的性质,对最终产物进行质谱分析,确定产物中含有-OH,确定3,7-二甲基-3-乙酰硫基-6-辛烯醛在硼氢化钠的催化下发生了还原反应。68791
毕业论文关键词:3,7-二甲基-3-乙酰硫基-6-辛烯醛;硼氢化钠;薄层层析;还原反应;图谱分析
The Reduction of 3,7-Dimethyl -3 -Acetylthio-6-Octenal by NaBH4
Abstract: The objective in this paper is to reduce the 3,7-dimethyl-3-acetylthio-6-octenal with NaBH4 which is used as the catalyst.After the reduction reaction,we need to isolate the product from the impurities and identify the production. The reduction reaction of 3,7-dimethyl-3-acetylthio-6-octenal with sodium borohydride is a warming reaction. First of all,we will set up a distillation device.Laying some 3,7-dimethyl-3 acetyl mercapto-6-octenal which is weighted into the flask with NaBH4.The weight on 3,7-dimethyl-3 acetyl mercapto-6-octenal and NaBH4 should be 2:1.Below the flask,we will add a beaker with ice as a ice bath device.After continuous stirring 2.5 to 3 hours,we can stop this reaction by adding 10 ml ice in the flask.The we use 15% dilute hydrochloric acid to adjust the pH to make sure the solution is neutral.With the end of the affirmance,we will set up a separation device to extract the solution with ethyl acetate.The organic layer will be washed by saturated sodium chloride for 2 to 3 times.Dried the organic layer with anhydrous sodium sulfate,then put the solution in some cool and dry place.One day later,use rotary steamer to distill the production.The product will be examined by using a chromatographic analysis.The final product was analyzed by mass spectrometry to determine whether the product contains -OH.If it contains,then prove the reduction action do happened.
Key Words: 3,7-dimethyl-3-acetylthio-6-octenal;sodium borohydride;thin-layer chromatography;reduction reaction;spectra analysis
目 录
1 背景 1
1.1硼氢化钠(NaBH4) 1
1.2还原反应 2
1.2.1 概念 2
1.2.2分类 2
(1)不饱和烃类的还原 2
(2)醇、酚的还原 6
(3)醛、酮的还原 7
(4)羧酸的还原 12
(5)酯及其衍生物的还原 12
(6)芳香族硝基化合物的还原 14
(7)卤代烃的还原反应 14
1.3含硫香料化合物 16
1.3.1综述