21080-80-8

基本信息
4-環(huán)丙基-2,4-氧代丁酸乙酯
4-環(huán)丙基-2,4-二氧代丁酸乙酯
4-環(huán)丙基-2,4-二羰基丁酸乙酯
4-環(huán)丙基-2,4-二氧代-丁酸乙酯
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thyl 4-cyclopropyl-2,4-dioxobutanoate
ethyl 4-cyclopropyl-2,4-dioxobutanoate
a,g-Dioxo-cyclopropanebutanoic acid ethyl ester
4-cyclopropyl-2,4-dioxo-butyric acid ethyl ester
4-cyclopropyl-2,4-dioxobutanoic acid ethyl ester
4-cyclopropyl-2,4-diketo-butyric acid ethyl ester
Cyclopropanebutanoic acid, α,γ-dioxo-, ethyl ester
物理化學(xué)性質(zhì)
常見問題列表

765-43-5

95-92-1

21080-80-8
在室溫和氮?dú)獗Wo(hù)下,將金屬鈉(16.19g)溶解于無水乙醇(150ml)中制備乙醇鈉溶液。將反應(yīng)混合物冷卻至0℃后,緩慢滴加草酸二乙酯(34.76g)和環(huán)丙甲基酮(20g)的混合液,滴加時(shí)間約為15分鐘。滴加完畢后,讓反應(yīng)混合物自然升溫至室溫。隨后,加入無水乙醇(100ml),并在室溫下繼續(xù)攪拌1小時(shí)。將反應(yīng)混合物加熱至80℃,維持45分鐘后冷卻至室溫,隨后在減壓條件下濃縮。向所得固體中加入乙酸乙酯,用乙醇洗滌后,通過布氏漏斗過濾,得到細(xì)粉末狀固體。將該固體溶解于水中,用稀硫酸調(diào)節(jié)pH至2進(jìn)行酸化。酸化后的溶液用乙醚萃取,有機(jī)相用無水硫酸鈉干燥,減壓濃縮后得到棕色液體狀目標(biāo)化合物4-環(huán)丙基-2,4-氧代丁酸乙酯(40g,收率93%)。
參考文獻(xiàn):
[1] Patent: WO2010/127855, 2010, A1. Location in patent: Page/Page column 159
[2] Patent: US2012/115903, 2012, A1. Location in patent: Page/Page column 40
[3] Patent: WO2012/62463, 2012, A1. Location in patent: Page/Page column 87-88
[4] Patent: WO2013/39988, 2013, A1. Location in patent: Page/Page column 138
[5] Patent: US2003/236287, 2003, A1. Location in patent: Page 46, 47