摘要
以1,3-戊二烯和溴代异丙基丙酮为原料,经过狄耳斯-阿德耳反应,得到产物脱溴化氢后,与乙醛反应,然后脱水,于减压下蒸馏,得到β-大马酮的立体异构体混合物。采用硅胶柱的多次柱层析分离,以石油醚和乙醚为洗脱剂,得到玫瑰香味的反式-β-大马酮产品,用IR,UV,NMR及MS光谱手段进行定性鉴定,用高压液相色谱进行定量测试,所得反式-β-大马酮含量可达94%。
Using penta-1, 3-diene and 3-bormo-mesityl oxide as starting materials, the mixture ofstereoisomers war obtained by a series of reactions: Diels-Alder reactiom dehydrobromination:acetaldehyde reaction; dehydration; and distillation under reduced pressure, The rose odoureddamascenone which was purified by repeated column chromatography using silica gel column andpetroleum and ether as eluants, was identified by IR, UV, NNR and MS; and its content wasdetermined by HPLC with a purity of up to 94%.
基金
国家自然科学基金
关键词
香料
大马酮
分离
光谱法
色谱法
Trans-β-Damascenone
IR
UV
~1H-NMR
^(13)C-NMR