105202-02-6

基本信息
3-Amino-4-iodobenzotrifluoride98%
3-Amino-4-iodobenzotrifluoride 98%
2-Iodo-5-(trifluoromethyl)aniline【3-Amino-4-iodobenzotrifluoride】
3-AMino-4-iodobenzotrifluoride[2-Iodo-5-(trifluoroMethyl)aniline]
2-Iodo-5-(trifluoromethyl)aniline, 6-Iodo-alpha,alpha,alpha-trifluoro-m-toluidine
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

400-97-5

105202-02-6
以3-硝基-4-碘三氟甲苯為原料合成2-碘-5-三氟甲基苯胺的一般步驟:在23℃條件下,向3-硝基-4-碘三氟甲苯(850mg,2.68mmol)的HOAc-EtOH混合溶液(10mL,體積比1:5)中加入鐵粉(750mg,13.43mmol)。將反應(yīng)混合物于23℃攪拌3小時(shí),隨后用飽和NaHCO3溶液(20mL)淬滅反應(yīng),并用EtOAc(50mL)稀釋。分離有機(jī)層和水層,有機(jī)層用去離子水(3×10mL)洗滌。合并的有機(jī)層經(jīng)無(wú)水Na2SO4干燥后,減壓濃縮。殘余物通過(guò)快速柱色譜法(硅膠為固定相,洗脫劑為己烷:EtOAc,體積比10:1)純化,得到2-碘-5-三氟甲基苯胺(754mg,收率98%)為黃色固體。1H NMR(400MHz,CDCl3)δ=7.76(dd,J=8.2,0.7Hz,1H),6.96(d,J=1.7Hz,1H),6.72(ddd,J=8.2,2.0,0.6Hz,1H),4.32(brs,2H)。質(zhì)譜(ESI)m/z:288.0 [M+H]+。
參考文獻(xiàn):
[1] Patent: WO2016/29310, 2016, A1. Location in patent: Paragraph 00357-00359
[2] Patent: US5079245, 1992, A
[3] Angewandte Chemie - International Edition, 2011, vol. 50, # 32, p. 7354 - 7358
[4] Patent: US5998334, 1999, A
[5] Organic Letters, 2017, vol. 19, # 17, p. 4484 - 4487