120511-72-0

基本信息
五甲基-1,3-二乙氰基苯
5,Α ,Α ,Α',Α'-五甲基-1,3-苯二乙腈
A,A,A',A',5-五甲基-1,3-苯二乙腈(阿那曲唑ANASTROZOLE中間體)
阿那曲唑中間體 1
2,2'-(5-methyl-1,3-phenylene)di(2-methylpropionitrile)
3,5-Bis(2-cyanoprop-2-yl)toluene
3,5-DI[(2,2-DIMETHYL)CYANOMETHYL]TOLUENE
5-PENTAMETHYL-1,3-BENZENEDIACETONITRILE
A,A,A',A',5-PENTAMETHYL-1,3 BENZENEDIACETONITRILE
PENTAMETHYL-1,3-BENZENEDIACETONITRILE
3,5-Bis (2-cyanoisopropyl ) toluene
2,2’-(5-Methyl-1,3-phenylene)-di(2-methylpropiononitrile
2,2'-(5-Methyl-1,3-Phenylene)Bis(2-Methylpropanenitrile)
2,2-(5-Methyl-1,3-Phenylene)-Bis-(2-Methyl-Propionitrile)
3,5-Bis(2-Cyanoisopropyl)Toluene(ForAnastrozole)
2,2-(5-methyl-1,3-phenylene)di(2-methylpropiononitrile (intermediate of anastrozole)
5-a,a,a',a'-Pentamethyl-1,3-Benzenediacetonitrile
-(5-Methyl-1,3-phenylene)-di(2-methylpropiononitrile
A,A,A'',A'',5-PENTAMETHYL1,3 BENZENEDIACETONITRIL
2-[3-(CYANO-DIMETHYL-METHYL)-5-METHYL-PHENYL]-2-METHYLPROPIONITRIL
2,2’-(5-Methyl-m-phenylene)bis-(2-methyl-propionitrile)
3,5-Bis(2-cyanoprop-2-yl)toluene 2,2'-(5-Methyl-1,3-phenylene)di(2-methylpropionitrile)a,a,a',a',5-Pentamethyl-1,3-benzenediacetonitrile
3,5-BIS(2-CYANOPROP-2-YL)TOLUENE,98%
物理化學(xué)性質(zhì)
制備方法

120511-74-2

74-88-4

120511-72-0
以2,2'-(5-甲基-1,3-亞苯基)二乙腈和碘甲烷為原料合成5,α,α,α',α'-五甲基-1,3-苯二乙腈的一般步驟:將3,5-雙(氰甲基)甲苯(800g,4.70mol)、甲基碘(2935.2g,20.68mol)和二甲基甲酰胺(11.20L)的混合物冷卻至0℃至5℃。在1至1.5小時內(nèi)分批加入60%氫化鈉在礦物油中的分散體(864.2g,36.0mol)。隨后,將反應(yīng)混合物逐漸升溫至室溫并持續(xù)攪拌2至2.5小時。反應(yīng)進程通過薄層色譜(TLC,展開劑為正己烷:乙酸乙酯=7.5:2.5)進行監(jiān)測。確認(rèn)反應(yīng)完成后,加入乙酸乙酯以淬滅過量的氫化鈉。將反應(yīng)混合物用水稀釋,并用二氯甲烷(3×5L)進行萃取。合并有機相,用鹽水(5L)洗滌。有機相在室溫下用活性炭脫色1小時,隨后在40℃至45℃下減壓濃縮至干。所得殘余物于70℃至75℃下溶解于四氯化碳(2400mL)中,并逐漸冷卻至10℃至15℃,攪拌1小時。進一步將溶液冷卻至-5℃至0℃,繼續(xù)攪拌3小時。最后,過濾攪拌的懸浮液,用預(yù)冷的四氯化碳(500mL)洗滌濾餅,并于40℃至45℃下真空干燥,得到3,5-雙(1-氰基-1-甲基乙基)甲苯(748.0g,產(chǎn)率70.3%)。
參考文獻:
[1] Organic and Biomolecular Chemistry, 2007, vol. 5, # 18, p. 2940 - 2952
[2] Patent: WO2006/836, 2006, A1. Location in patent: Page/Page column 2; 9-10; 14; Figure 2
[3] Patent: US2006/189670, 2006, A1. Location in patent: Page/Page column 5-7
[4] Patent: WO2007/39913, 2007, A1. Location in patent: Page/Page column 13-14
[5] Patent: US2008/207915, 2008, A1. Location in patent: Page/Page column 5