42186-06-1
42186-06-1 結構式
基本信息
2-(4-BroMo-phenyl)-propionitrile
Benzeneacetonitrile, 4-bromo-α-methyl-
物理化學性質(zhì)
制備方法
16532-79-9
74-88-4
42186-06-1
實施例649 2-(4-溴苯基)丙腈的合成:將2-(4-溴苯基)乙腈(5.0 g,25.5 mmol)溶于無水THF(70 mL)中,冷卻至0℃。在攪拌下分批加入氫化鈉(60 wt%,1.5 g,38.3 mmol)。反應混合物在室溫下攪拌1小時。隨后,加入甲基碘(1.8 mL,28.1 mmol),繼續(xù)攪拌14小時。反應完成后,小心地在0℃下用水淬滅反應,并用乙酸乙酯(200 mL)稀釋。分離有機層,用無水硫酸鈉干燥,過濾后濃縮。殘余物通過柱色譜法(硅膠,0-30%乙酸乙酯/庚烷梯度洗脫)純化,得到目標產(chǎn)物2-(4-溴苯基)丙腈(3.8 g,72%),為黃色油狀物。ESI MS m/z 210 [C9H8BrN + H]+。
參考文獻:
[1] Journal of the American Chemical Society, 2015, vol. 137, # 19, p. 6156 - 6159
[2] Patent: WO2011/123419, 2011, A1. Location in patent: Page/Page column 386
[3] Patent: WO2017/139778, 2017, A1. Location in patent: Paragraph 00487
[4] Patent: US2013/331375, 2013, A1. Location in patent: Paragraph 0178
[5] Patent: WO2018/140876, 2018, A1. Location in patent: Page/Page column 113; 115
