1027345-07-8
1027345-07-8 結(jié)構(gòu)式
基本信息
4-fluoro-3-(trifuoromethylsulfonyl)benzenesulfonyl chlo
4-Fluoro-3-(trifluoromethylsulfonyl)benzenesulfonyl Chloride
4-Fluoro-3-[(trifluoromethyl)sulphonyl]benzenesulphonyl chloride
Benzenesulfonyl chloride, 4-fluoro-3-[(trifluoromethyl)sulfonyl]-
4-fluoro-3-((trifluoroMethyl)sulfonyl)benzene-1-sulfonyl chloride
物理化學(xué)性質(zhì)
制備方法
2358-41-0
1027345-07-8
以1-氟-2-(三氟甲磺?;?苯為原料合成3-(三氟甲基磺?;?-4-氟苯磺酰氯的一般步驟:將1-氟-2-(三氟甲磺?;?苯(10.00g,43.83mmol)溶解于氯磺酸(35.00mL)中,在120℃下加熱反應(yīng)5小時(shí)。反應(yīng)完成后,將混合物緩慢倒入由碎冰(100g)和水(300mL)組成的混合液中。用二氯甲烷(80mL×2)萃取反應(yīng)混合物,合并有機(jī)相后用蒸餾水(200mL×2)洗滌。有機(jī)相經(jīng)無(wú)水硫酸鈉干燥后,減壓濃縮,得到3-(三氟甲基磺?;?-4-氟苯磺酰氯(12.60g,38.57mmol,收率88%),該產(chǎn)物無(wú)需進(jìn)一步純化即可用于下一步反應(yīng)。質(zhì)譜(ESI)m/z = 307 [M-Cl+OH-H]。1H NMR(400MHz,DMSO-d6):δ8.25(m,1H),8.15(m,1H),7.73(m,1H)。
參考文獻(xiàn):
[1] Patent: WO2017/101851, 2017, A1. Location in patent: Paragraph 0135; 0138
[2] Patent: WO2008/61208, 2008, A2. Location in patent: Page/Page column 30-31
[3] Synthesis, 2008, # 15, p. 2398 - 2404
[4] Journal of Medicinal Chemistry, 2008, vol. 51, # 21, p. 6902 - 6915
[5] Patent: US2009/318689, 2009, A1. Location in patent: Page/Page column 34