89720-77-4

基本信息
4-溴-1-(溴甲基)-2-氯苯
Benzene, 4-bromo-1-(bromomethyl)-2-chloro-
安全數(shù)據(jù)
制備方法

185315-48-4

89720-77-4
在氬氣保護(hù)和0℃條件下,向(4-溴-2-氯苯基)甲醇(2.80 g,12.67 mmol)的二氯甲烷(60.0 mL)溶液中依次加入四溴化碳(4.41 g,13.30 mmol)和三苯基膦(3.48 g,13.30 mmol)。將反應(yīng)混合物在室溫下攪拌4小時(shí)。反應(yīng)完成后,將混合物減壓濃縮,所得粗產(chǎn)物通過(guò)快速柱色譜法(洗脫劑:10%乙酸乙酯的己烷溶液)純化,得到2-氯-4-溴溴芐,為無(wú)色油狀物(3.59 g,收率100%)。1H NMR(400 MHz,CDCl3):δ 4.53(s,2H),7.29(d,J = 8.2 Hz,1H),7.39(dd,J = 8.2, 1.9 Hz,1H),7.56(d,J = 1.9 Hz,1H)。
參考文獻(xiàn):
[1] Patent: WO2004/74270, 2004, A2. Location in patent: Page 175
[2] Patent: WO2006/18725, 2006, A1. Location in patent: Page/Page column 235-236
[3] Patent: WO2008/18827, 2008, A1. Location in patent: Page/Page column 65-66
[4] Patent: WO2010/15652, 2010, A2. Location in patent: Page/Page column 68
[5] Tetrahedron Letters, 2016, vol. 57, # 3, p. 449 - 451