化学合成。
化学合成
合成路线 1(1. 合成:6214-44-4)
产率:82%
合成条件:With sodium tetrahydroborate In methanol at 0 - 20℃; for 0.75 h;
实验步骤:在0℃下,将NaBH 4(0.8g,21.7mmol)加入到搅拌的4-乙氧基苯甲醛(3.0g,19.7mmol)的甲醇(50ml)溶液中,历时15分钟,并将反应混合物在环境温度下搅拌30分钟。 温度。 蒸发溶剂,得到残余物,将其溶于水中,用EtOAc萃取两次。 将合并的有机萃取液用水和盐水洗涤,用硫酸钠干燥,并减压浓缩,得到(4-乙氧基苯基)甲醇,产率82%。 LC / MS [M + H] 135.2。 1H-NMR(400MHz,CDCl3)δ7.266-7.286(d,2H,J = 8.0Hz),6.872-6.893(d,2H,J = 8.4Hz),4.609(s,2H),4.010-4.061(q ,2H,J = 6.8Hz),1.396-1.430(t,3H,j = 6.8Hz)。
参考文献:
- [1] Advanced Synthesis and Catalysis, 2016, vol. 358, # 10, p. 1694 - 1698 [2] Patent: WO2010/127208, 2010, A1. Location in patent: Page/Page column 62 [3] Journal of Medicinal Chemistry, 2017, vol. 60, # 12, p. 4861 - 4868 [4] Justus Liebigs Annalen der Chemie, 1933, vol. 507, p. 1,9 [5] Journal of the Chemical Society, 1956, p. 2455,246 [6] Journal of the Chemical Society, 1954, p. 2351 [7] Bioorganic and Medicinal Chemistry Letters, 2001, vol. 11, # 16, p. 2205 - 2208 [8] Patent: US5248825, 1993, A [9] Electrochimica Acta, 2012, vol. 59, p. 270 - 278 [10] Catalysis Today, 2015, vol. 247, p. 14 - 19 [11] Bioorganic and Medicinal Chemistry, 2018, vol. 26, # 12, p. 3145 - 3157