22227-63-0
22227-63-0 結(jié)構(gòu)式
基本信息
3-Nitro-5-trifluoromethyl-benzoic acid methyl ester
常見問題列表
67-56-1
328-80-3
22227-63-0
將3-硝基-5-(三氟甲基)苯甲酸（1g，4.25mmol）溶解于甲醇（15mL）中，加入濃硫酸（5滴）作為催化劑。將反應(yīng)混合物加熱回流48小時(shí)。反應(yīng)完成后，減壓蒸餾除去甲醇。將殘余物溶解于乙酸乙酯（20mL）中，依次用5%碳酸鈉溶液（3×20mL）和飽和食鹽水（20mL）洗滌。有機(jī)層經(jīng)無水硫酸鈉干燥后，減壓濃縮，得到3-硝基-5-三氟甲基苯甲酸甲酯，無需進(jìn)一步純化。產(chǎn)率為87%，產(chǎn)物為無色油狀物。1H NMR (500 MHz, CDCl3) δ 9.05 (t, J = 1.8 Hz, 1H), 8.68 (t, J = 1.8 Hz, 1H), 8.63 (s, 1H), 4.05 (s, 3H). 13C NMR (126 MHz, CDCl3) δ 163.62, 148.47, 133.16, 132.83 (q, J = 34.7 Hz), 131.87 (q, J = 3.5 Hz), 127.50, 124.42 (q, J = 3.8 Hz), 122.37 (q, J = 273.2 Hz), 53.26.
參考文獻(xiàn)：
[1] Patent: WO2012/37132, 2012, A1. Location in patent: Page/Page column 47
[2] Patent: US2012/71489, 2012, A1. Location in patent: Page/Page column 59
[3] Patent: WO2017/125530, 2017, A1. Location in patent: Page/Page column 283
[4] Bioorganic and Medicinal Chemistry, 2006, vol. 14, # 12, p. 4158 - 4181
[5] Patent: WO2014/141187, 2014, A1. Location in patent: Page/Page column 119