【摘要】 研究了2,7-二甲基-2,4,6-辛三烯-1,8-二醛并联合成工艺,以4-乙酰氧基-2-甲基-2-丁烯醛为原料,经醛基保护、酯交换、氧化合成3-(5,5-二甲基-1,3-二噁烷-2-基)-2-丁烯醛;采用氯化亚铜、1-氧自由基-2,2,6,6-四甲基-4-羟基-哌啶催化氧化2-(3-羟基-1-甲基-1-丙烯基)-5,5-二甲基-1,3-二噁烷合成3-(5,5-二甲基-1,3-二噁烷-2-基)-2-丁烯醛;2-(3-羟基-1-甲基-1-丙烯基)-5,5-二甲基-1,3-二噁烷经过氯化合成2-(3-氯-1-甲基-1-丙烯基)-5,5-二甲基-1,3-二噁烷;3-(5,5-二甲基-1,3-二噁烷-2-基)-2-丁烯醛、2-(3-氯-1-甲基-1-丙烯基)-5,5-二甲基-1,3-二噁烷与亚磷酸三乙酯一锅法工艺制得十碳三烯双醛,以五碳醛作为基准物,并联工艺总收率为48%.更多还原

【Abstract】 A parallel process for the new synthesis of 2,7-dimethyl-2,4,6-octatriene-1,8-dial was investigated.3-（5,5-Dimethyl-1,3-dioxan-2-yl）-2-butenal was obtained by a process involving aldehyde protection,ester exchange and catalytic oxidation from 4-acetoxy-2-methyl-2-butenal.A new catalytic oxidation process was proposed to get 3-（5,5-dimethyl-1,3-dioxan-2-yl）-2-butenal by oxidating 3-（5,5-dimethyl-1,3-dioxan-2-yl）-2-buten-1-ol with copper（Ⅰ） chloride、2,2,6,6-tetramethyl-1-piperidinyloxy and oxygen.3-（5,5-Dimethyl-1,3-dioxan-2-yl）-2-buten-1-ol was chlorizated with SOCl₂ in DMF to get 2-（3-chloro-1-methyl-1-propenyl）-5,5-dimethyl-1,3-dioxane.2,7-Dimethyl-2,4,6-octatriene-1,8-dial was acquired in an overall yield of 48% by one-pot synthesis method from 3-（5,5-dimethyl-1,3-dioxan-2-yl）-2-butenal,2-（3-chloro-1-methyl-1-propenyl）-5,5-dimethyl-1,3-dioxane and triethylphosphite.更多还原