34916-10-4

基本信息
4-氧代環(huán)己烷甲腈
4-氧代-環(huán)己甲腈
4-Isocyanocyclohexanone, 99%
4-OXOCYCLOHEXANECARBONITRILE
4-oxocyclohexane-1-carbonitrile
CYCLOHEXANECARBONITRILE, 4-OXO-
4-oxo-1-cyclohexanecarbonitrile
4-OXOCYCLOHEXANECARBONITRILE(WXC05700)
物理化學(xué)性質(zhì)
制備方法
![1,4-二氧雜螺[4.5]癸烷-8-甲腈](/CAS/GIF/69947-09-7.gif)
69947-09-7

34916-10-4
以1,4-二氧雜螺[4.5]癸烷-8-甲腈為原料合成4-氧代環(huán)己烷甲腈的一般步驟如下:在5000 mL三頸燒瓶中加入1,4-二氧雜螺[4.5]癸烷-8-甲腈200.6 g(1.2 mol)、硼酸72 g(1.2 mol)、水2000 mL(10體積當(dāng)量)和鹽酸。隨后加入1000 mL(5體積當(dāng)量)四氫呋喃和500 mL(2.5體積當(dāng)量)水,將混合物加熱至60℃,反應(yīng)持續(xù)2小時。反應(yīng)過程中取樣,通過氣相色譜(GC)監(jiān)測反應(yīng)進(jìn)度。當(dāng)剩余原料量低于2%時,視為反應(yīng)完成。將反應(yīng)混合物冷卻至室溫后,加入二氯甲烷進(jìn)行萃取,重復(fù)三次。合并二氯甲烷層,通過減壓蒸餾除去溶劑。最后,對產(chǎn)物進(jìn)行精餾,條件為100℃、2 mmHg,得到4-氧代環(huán)己烷甲腈140.4 g,GC純度為98%,收率為95%。
參考文獻(xiàn):
[1] Patent: CN108329234, 2018, A. Location in patent: Paragraph 0018-0022
[2] Patent: WO2007/13848, 2007, A1. Location in patent: Page/Page column 8-9
[3] Patent: EP3124482, 2017, A1. Location in patent: Paragraph 0211; 0213
[4] Patent: WO2007/50612, 2007, A1. Location in patent: Page/Page column 116-117
[5] Patent: WO2009/156100, 2009, A1. Location in patent: Page/Page column 156