197846-82-5

基本信息
4-(3-溴苯基)嗎啉
1-溴-3-(4-嗎啉-4-基)苯
N-(3-BroMophenyl)Morpholine
1-(3-bromophenyl)-morpholine
Morpholine,4-(3-broMophenyl)-
4-(3-Bromophenyl)morpholine96%
1-BROMO-3-(4-MORPHOLINO)BENZENE
4-(3-Bromophenyl)morpholine 96%
1-Bromo-3-(morpholin-4-yl)benzene
物理化學(xué)性質(zhì)
制備方法

110-91-8

108-36-1

197846-82-5
以1,3-二溴苯(50g,0.21mol)和嗎啉(15.89mL,0.19mol)為原料,在氬氣保護下,將兩者與無水甲苯(200mL)通過注射器加入反應(yīng)燒瓶中。充分混合后,依次加入R-BINAP(1.32g,0.0021mol)、二亞芐基丙酮鈀(0)(0.640g,0.006mol)和DBU(25.8mL,0.17mol)。將反應(yīng)混合物在60℃下攪拌,隨后加入叔丁醇鈉(30.55g,0.32mol),并將反應(yīng)溫度升至100℃,持續(xù)反應(yīng)過夜。反應(yīng)完成后,將懸浮液用乙酸乙酯稀釋,通過硅藻土過濾,依次用水和鹽水洗滌有機相。有機相經(jīng)無水硫酸鎂干燥后,減壓濃縮除去溶劑。粗產(chǎn)物通過硅膠柱色譜純化,洗脫劑為乙酸乙酯:己烷(1:1),得到目標(biāo)化合物4-(3-溴苯基)嗎啉,為黃色油狀物(36.5g,收率71%)。質(zhì)譜(ES+)顯示分子離子峰m/z 242([M+H]+)。
參考文獻(xiàn):
[1] Patent: WO2011/144578, 2011, A1. Location in patent: Page/Page column 28
[2] Journal of Medicinal Chemistry, 2015, vol. 58, # 14, p. 5522 - 5537
[3] Tetrahedron, 2008, vol. 64, # 13, p. 2938 - 2950
[4] Patent: WO2011/144577, 2011, A1. Location in patent: Page/Page column 25-26