83922-51-4

基本信息
N-(3-溴苯基)甲烷磺酰胺
3-(methylsulfonyl)amino-1-bromo-benzene
物理化學(xué)性質(zhì)
制備方法

124-63-0

591-19-5

83922-51-4
步驟i:在10℃下,向攪拌的間溴苯胺(6g,34.87mmol)的無(wú)水二氯甲烷(200ml)溶液中依次加入吡啶(4.13mg,52.31mmol)和甲基磺酰氯(5.194g,45.34mmol)。反應(yīng)混合物在室溫下攪拌15小時(shí),反應(yīng)進(jìn)程通過(guò)薄層色譜(TLC,展開劑為35%乙酸乙酯的己烷溶液)監(jiān)測(cè)。反應(yīng)完成后,用二氯甲烷(50ml)稀釋反應(yīng)混合物,并用1N鹽酸(25ml)洗滌。有機(jī)層用無(wú)水硫酸鈉干燥,減壓濃縮,得到N-(3-溴苯基)甲烷磺酰胺8.45g,收率96.3%。產(chǎn)物經(jīng)1H NMR(DMSO-d6,300MHz)和質(zhì)譜(MS:m/z = 251.8 [M + 1])確認(rèn)結(jié)構(gòu)。
參考文獻(xiàn):
[1] Patent: WO2014/6554, 2014, A1. Location in patent: Page/Page column 28
[2] Synthetic Communications, 2004, vol. 34, # 20, p. 3807 - 3819
[3] Patent: WO2017/18803, 2017, A1. Location in patent: Paragraph 791; 792; 793
[4] Spectrochimica Acta, Part A: Molecular and Biomolecular Spectroscopy, 1982, vol. 38, # 7, p. 791 - 796
[5] Heterocycles, 2001, vol. 54, # 1, p. 105 - 108