摘要
氯异戊烯与亚异丙基丙酮在相转移催化条件下缩合得2和3,以氢氧化钠代替 DBU 在分馏塔内使副产物3异构化为2,并对缩合的条件进行了研究,2经格氏、重排及氢化等反应得六氢假紫罗酮(1),纯度98%,总收率43.4%。
3-Methyl-2-butenyl chloride reacted with mesityl oxide underphasetransfer catalylic condition to give 61% 3-isopropenyl-6-methyl-5-hepten-2-one(2)and 22% 3-isopropylidene-6-methyl-5-hepten-2-one(3),which could be isomerizedto 2 in 88% yield by continuous fractional distillation in the presence of sodiumhydroxide.Grignard reaction of 2 gave 79% yield of 4,which under thermolysis inN-methyl-2-pyrrolidone afforded 74% yield of 6,10-dimethyl-6,9-undecadien-2-one(5),which was hydrogenated with Pd/C to give hexahydropseudoionone of 98%purity in 92% yield.
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
1991年第2期54-57,共4页
Chinese Journal of Pharmaceuticals
关键词
六氢假紫罗酮
合成
hexahydropseudoionone
PTC
Oxy-Cope
rearrangement
catalytic hydrogenation
synthesis
