20249-16-5

基本信息
3-氧代環(huán)丁烷甲腈
3-氧代-環(huán)丁基甲腈
3-OXO-CYCLOBUTANECARBONITRILE
Cyclobutanecarbonitrile, 3-oxo-
3-oxocyclobutane-1-carbonitrile
物理化學(xué)性質(zhì)
制備方法

15760-35-7

20249-16-5
實(shí)施例37b 3-氧代環(huán)丁烷甲腈的合成:在5℃下,將偏高碘酸鈉(284g,1.32mol)分小批(30-45分鐘內(nèi))加入到3-亞甲基環(huán)丁烷甲腈(30g,370mmol)和三氯化釕一水合物(2.2mol%,1.5g,7.23mmol)在DCM-MeCN-水(645mL:645mL:945mL)的混合溶劑中。反應(yīng)混合物在室溫下劇烈攪拌。隨后,分離有機(jī)相,水相用DCM(3×1500mL)萃取。合并的有機(jī)萃取物通過快速硅膠小墊過濾,硅膠墊用2000mL DCM洗滌。濾液用MgSO4干燥,過濾并減壓濃縮,得到3-氧代環(huán)丁烷甲腈(28g,100%)。產(chǎn)物經(jīng)1H NMR(400MHz,CDCl3)表征:δ 3.27(quin,1H),3.57(d,4H)。
參考文獻(xiàn):
[1] Patent: US2012/122843, 2012, A1. Location in patent: Page/Page column 39
[2] Patent: WO2015/179190, 2015, A1. Location in patent: Paragraph 0331
[3] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 13, p. 3947 - 3953
[4] Patent: US2014/80803, 2014, A1. Location in patent: Paragraph 1262
[5] Journal of Medicinal Chemistry, 2016, vol. 59, # 10, p. 4926 - 4947