172023-97-1

基本信息
3-溴-5-(三氟甲基)苯甲醇
3-BROMO-5-(TRIFLUOROMETHYL)BENZYL ALCOHOL
3-Bromo-5-(trifluoromethyl)benzenemethanol
[3-BROMO-5-(TRIFLUOROMETHYL)PHENYL]METHANOL
Benzenemethanol, 3-bromo-5-(trifluoromethyl)-
3-Bromo-5-(trifluoromethyl)benzyl alcohol 98%
(3-Bromo-5-(trifluoromethyl)phenyl)methanol M61623
物理化學(xué)性質(zhì)
制備方法

537039-44-4

172023-97-1
以(3-氨基-5-(三氟甲基)苯基)甲醇為原料合成3-溴-5-(三氟甲基)芐醇的一般步驟:將(3-氨基-5-(三氟甲基)苯基)甲醇(1.6 g,8.4 mmol)溶解于無水乙腈(10 mL)中,緩慢滴加至含有溴化銅(II)(2.24 g,10.0 mmol)和叔丁基亞硝酸鹽(1.48 mL,12.0 mmol)的乙腈(20 mL)溶液中。反應(yīng)混合物在65℃下攪拌30分鐘后,冷卻至室溫,倒入1N鹽酸溶液中,并用乙酸乙酯(2×)進(jìn)行萃取。合并有機(jī)層,用鹽水(2×)洗滌,經(jīng)無水硫酸鈉干燥后濃縮。通過硅膠柱色譜(20%乙酸乙酯/己烷)純化,得到目標(biāo)產(chǎn)物3-溴-5-(三氟甲基)芐醇(1.48 g,產(chǎn)率69%)。1H-NMR(CDCl3, 500 MHz)δ 7.71(s, 1H),7.68(s, 1H),7.55(s, 1H),4.75(s, 2H)。
參考文獻(xiàn):
[1] Patent: US2007/249607, 2007, A1. Location in patent: Page/Page column 62
[2] Bioorganic and Medicinal Chemistry Letters, 2015, vol. 25, # 15, p. 3039 - 3043
[3] Patent: WO2007/88999, 2007, A1. Location in patent: Page/Page column 164-165
[4] Patent: WO2007/116922, 2007, A1. Location in patent: Page/Page column 54
[5] Patent: WO2005/100298, 2005, A1. Location in patent: Page/Page column 65