466639-53-2

基本信息
2-溴-4-甲氧基碘苯
1-碘-2-溴-4-甲氧基苯
2-溴-1-碘-4-甲氧基苯
2 - 溴-1-碘-4-苯甲醚
2-BROMO-1-IODO-5-METHOXYBENZENE
3-Bromo-4-iodoanisole97%
3-Bromo-4-iodoanisole 97%
2-bromo-1-iodo-4-methoxybenzene
Benzene, 2-bromo-1-iodo-4-methoxy-
2-Bromo-1-iodo-4-methoxybenzene, 3-Bromo-4-iodophenyl methyl ether
物理化學(xué)性質(zhì)
制備方法

2398-37-0

466639-53-2
以3-溴茴香醚為起始原料合成2-溴-1-碘-4-甲氧基苯的一般步驟:在攪拌條件下,將3-溴茴香醚(10g,53.5mmol)、氧化汞(HgO,8.8g,40.6mmol)和乙酸酐(Ac2O,1mL)溶于二氯甲烷(CH2Cl2,100mL)中,回流30分鐘。隨后,分6次每隔12小時(shí)加入碘(I2,17.6g,69.5mmol),每次加入后繼續(xù)回流12小時(shí)。反應(yīng)完成后,通過硅藻土墊過濾反應(yīng)混合物,濾液用飽和硫代硫酸鈉(Na2S2O3)溶液洗滌。水層用二氯甲烷(3×10mL)萃取,合并有機(jī)層,用無水硫酸鎂(MgSO4)干燥,隨后減壓濃縮至干。通過快速柱色譜法(以環(huán)己烷為洗脫劑)純化粗產(chǎn)物,得到目標(biāo)化合物2-溴-1-碘-4-甲氧基苯,為無色油狀物(產(chǎn)率94%)。產(chǎn)物經(jīng)1H NMR(300MHz,CDCl3)表征:δ 7.68(d,J = 8.8Hz,1H),7.19(d,J = 2.8Hz,1H),6.59(dd,J = 2.8Hz,J = 8.8Hz,1H),3.77(s,3H)。
參考文獻(xiàn):
[1] European Journal of Medicinal Chemistry, 2010, vol. 45, # 9, p. 3617 - 3626
[2] Patent: WO2015/121785, 2015, A1. Location in patent: Page/Page column 39; 41
[3] Journal of the American Chemical Society, 2012, vol. 134, # 22, p. 9291 - 9295
[4] Chemical Communications, 2017, vol. 53, # 44, p. 5970 - 5973
[5] Organic and Biomolecular Chemistry, 2018, vol. 16, # 38, p. 7019 - 7028