83265-53-6

220107-65-3

以2-氨基-5-三氟甲基苯甲酸為原料合成(2-氨基-5-(三氟甲基)苯基)甲醇的一般步驟如下：首先，根據(jù)文獻方法由化合物22b制備化合物24a，進而合成目標產(chǎn)物28b。該步驟的產(chǎn)率為84%，產(chǎn)物為黃色無定形固體。通過紅外光譜(IR, KBr)檢測，主要吸收峰位于3389, 2918, 1461, 1274, 1122 cm-1。核磁共振氫譜(1H NMR, 300 MHz, CDCl3)顯示δ值：1.26-1.34 (1H, m), 2.09 (1H, dt, J = 5.1, 12.6 Hz), 2.27 (1H, dt, J = 2.4, 12.0 Hz), 2.39-2.50 (1H, m), 2.43 (3H, s), 2.89 (1H, d, J = 6.3 Hz), 2.96-2.99 (2H, m), 3.08 (1H, d, J = 17.7 Hz), 3.27 (1H, d, J = 17.7 Hz), 3.49 (1H, d, J = 17.4 Hz), 3.69 (1H, d, J = 17.7 Hz), 6.68 (1H, dd, J = 2.1, 8.3 Hz), 7.01 (2H, d, J = 8.3 Hz), 7.04 (1H, d, J = 2.1 Hz), 7.28 (1H, d, J = 8.3 Hz), 7.58 (1H, s), 7.63 (1H, s)，其中兩個質(zhì)子(OH)未觀察到。核磁共振碳譜(13C NMR, 75 MHz, CDCl3)顯示δ值：23.9, 35.8, 36.1, 38.8, 40.3, 42.9, 45.4, 61.5, 69.3, 113.1, 115.2, 123.78 (q, J = 270.5 Hz), 123.79 (q, J = 3.1 Hz), 124.5 (q, J = 4.3 Hz), 125.7, 126.8, 127.0 (q, J = 32.3 Hz), 127.7, 129.0, 129.9, 136.6, 140.4, 145.9, 155.4, 160.0。高分辨質(zhì)譜(HRMS, ESI)顯示：[M + H]+的計算值為C25H24F3N2O2，441.1790；實測值為441.1775。

參考文獻：

[1] Bioorganic and Medicinal Chemistry, 2012, vol. 20, # 19, p. 5810 - 5831

[2] Patent: US6369221, 2002, B1. Location in patent: Page column 37