68432-92-8

基本信息
3-氰基甲基苯甲酸甲酯
3-(氰基乙基)苯甲酸甲酯
Methyl m-(cyanomethyl)benzoate
3-CYANOMETHYLBENZOIC ACID METHYL ESTER
Benzoicacid, 3-(cyanomethyl)-, methyl ester
high quality 3-CYANOMETHYLBENZOIC ACID METHYL ESTER
物理化學(xué)性質(zhì)
制備方法

143-33-9

1129-28-8

68432-92-8
以氰化鈉和3-溴甲基苯甲酸甲酯為原料合成間氰甲基苯甲酸甲酯的一般步驟如下:將3-溴甲基苯甲酸甲酯(13.5 g,58.9 mmol)和氰化鈉(4.33 g,88.4 mmol)懸浮于N,N-二甲基甲酰胺(DMF,25 mL)和水(1 mL)的混合溶劑中,于75℃下攪拌反應(yīng)5小時。反應(yīng)完成后,用去離子水(50 mL)淬滅反應(yīng),并以乙酸乙酯(EtOAc,100 mL×3)進(jìn)行萃取。合并有機(jī)相,經(jīng)無水硫酸鈉干燥后,減壓濃縮除去溶劑。所得粗產(chǎn)物通過ISCO系統(tǒng)(洗脫劑:正己烷-乙酸乙酯梯度)進(jìn)行柱色譜純化,最終得到7.2 g(產(chǎn)率70%)目標(biāo)產(chǎn)物間氰甲基苯甲酸甲酯,為無色油狀物。核磁共振氫譜(NMR)數(shù)據(jù)如下:δ 7.90(s,1H),7.86(d,1H),7.60(d,1H),7.50(m,1H),4.10(s,2H),3.80(s,3H);質(zhì)譜(m/z):175。
參考文獻(xiàn):
[1] Patent: WO2006/67446, 2006, A1. Location in patent: Page/Page column 126
[2] Patent: WO2006/79791, 2006, A1. Location in patent: Page/Page column 34
[3] Patent: WO2006/24834, 2006, A1. Location in patent: Page/Page column 63-64
[4] Patent: WO2006/24836, 2006, A1. Location in patent: Page/Page column 27
[5] Patent: WO2007/71955, 2007, A1. Location in patent: Page/Page column 50-51