22446-38-4 2-(3-羟基苯基)乙酸乙酯

运输信息：常温运输。危险描述：非危险化学品，海关编码2918290090。

化学合成；3-羟基苯乙酸乙酯是制备新型抗炎药的有效合成中间体。

医药

路线1：

• 步骤: 将（3-羟基 - 苯基） - 乙酸（10g，65.7mmol）溶于EtOH（50mL）中，加入催化量的亚硫酰氯（~0.5mL），室温搅拌6小时，真空除去溶剂得到产物。
• 条件: 20℃；6小时
• 收率: 100%
• 参考文献: [1] Patent: WO2007/56366, 2007, A2. Location in patent: Page/Page column 26 [2] Patent: WO2007/56497, 2007, A1. Location in patent: Page/Page column 22 [3] Patent: WO2011/44394, 2011, A1. Location in patent: Page/Page column 127-128 [4] Journal of Medicinal Chemistry, 2012, vol. 55, #14, p. 6427 - 6437 [5] Bioorganic and Medicinal Chemistry Letters, 2011, vol. 21, #1, p. 299 - 302 [6] Journal of Chemical Research, 2016, vol. 40, #8, p. 506 - 510 [7] Bioorganic and Medicinal Chemistry, 2010, vol. 18, #22, p. 8092 - 8105 [8] Patent: WO2008/145678, 2008, A1. Location in patent: Page/Page column 41-42 [9] Journal of Medicinal Chemistry, 1997, vol. 40, #7, p. 1049 - 1062 [10] Tetrahedron Letters, 1993, vol. 34, #52, p. 8549 - 8552 [11] Tetrahedron, 1994, vol. 50, #41, p. 11945 - 11966 [12] Tetrahedron Asymmetry, 1995, vol. 6, #6, p. 1345 - 1356 [13] Tetrahedron, 1996, vol. 52, #42, p. 13493 - 13512 [14] Patent: US2009/156590, 2009, A1. Location in patent: Page/Page column 40; 49; 52-53 [15] Bioorganic and Medicinal Chemistry, 2016, vol. 24, #21, p. 5340 - 5352 [16] Journal of Medicinal Chemistry, 2007, vol. 50, #7, p. 1495 - 1503 [17] Tetrahedron Letters, 1992, vol. 33, #27, p. 3919 - 3922 [18] Bioorganic and Medicinal Chemistry Letters, 2005, vol. 15, #23, p. 5274 - 5279 [19] Journal of Medicinal Chemistry, 2005, vol. 48, #23, p. 7153 - 7165 [20] Journal of Organic Chemistry, 2001, vol. 66, #23, p. 7818 - 7824 [21] Patent: EP1422224, 2004, A1. Location in patent: Page 21 [22] Patent: WO2007/56771, 2007, A2. Location in patent: Page/Page column 37; 39 [23] Bioorganic and Medicinal Chemistry Letters, 2018, vol. 28, #14, p. 2539 - 2542 [24] Patent: WO2006/127133, 2006, A2. Location in patent: Page/Page column 44 [25] Patent: WO2007/146768, 2007, A2. Location in patent: Page/Page column 10 [26] Patent: WO2009/102893, 2009, A2. Location in patent: Page/Page column 95 [27] Patent: WO2009/145989, 2009, A2. Location in patent: Page/Page column 104 [28] Patent: WO2009/151695, 2009, A1. Location in patent: Page/Page column 71-72 以乙醇和3-羟基苯基乙酸为原料合成2-(3-羟基苯基)乙酸乙酯（S16-2）的一般步骤：向3-羟基苯基乙酸（S16-1; 10g，65.8mmol）的200mL乙醇溶液中加入8mL浓硫酸，加热回流过夜。反应完成后，减压浓缩反应混合物，残余物溶解于乙酸乙酯，用蒸馏水洗涤，合并有机层，饱和食盐水洗涤，无水硫酸镁干燥，过滤后蒸发溶剂得粗产物，经快速柱色谱法纯化得无色油状目标化合物，收率定量。产物结构经1H NMR（500MHz，CDCl3）确认：δ7.35（br，1H），7.12（m，1H），6.69-6.78（m，3H），4.12（m，2H），3.53（s，2H），1.21（m，3H）。 参考文献：[1] Patent: WO2007/56366, 2007, A2. Location in patent: Page/Page column 26 [2] Patent: WO2007/56497, 2007, A1. Location in patent: Page/Page column 22 [3] Patent: WO2011/44394, 2011, A1. Location in patent: Page/Page column 127-128