化学合成。
化学合成
合成路线 1(1. 合成:28539-02-8)
产率:94%
合成条件:at 25℃; for 0.08 h;
实验步骤:实施例30 1-羟基甲基-1H-苯并三唑将10g(83.94mmol)1H-苯并三唑溶于6.81mL(83.94mmol)37%甲醛水溶液中。 搅拌并使混合物达到25℃的温度.5分钟后,反应混合物固化。 将溶液冷却至环境温度。 过滤并用乙醚洗涤。 将残余物在冷的四氢呋喃中研磨并过滤(Int.94)。 产率:94%熔点:148-150℃(四氢呋喃和乙醚)
参考文献:
- [1] Patent: US2004/67998, 2004, A1. Location in patent: Page/Page column 24 [2] Journal of the American Chemical Society, 2017, vol. 139, # 27, p. 9281 - 9290 [3] Patent: CN102688233, 2016, B. Location in patent: Paragraph 0095; 0098 [4] Patent: CN106188103, 2016, A. Location in patent: Paragraph 0035; 0037 [5] Journal of the American Chemical Society, 1952, vol. 74, p. 3868 [6] Justus Liebigs Annalen der Chemie, 1934, vol. 511, p. 213,240 [7] Recueil des Travaux Chimiques des Pays-Bas, 1988, vol. 107, # 11, p. 641 - 646 [8] Journal of Organic Chemistry, 1989, vol. 54, # 26, p. 6022 - 6029 [9] Bioorganic and Medicinal Chemistry Letters, 1997, vol. 7, # 15, p. 2009 - 2014 [10] Organic Preparations and Procedures International, 1992, vol. 24, # 4, p. 475 - 478 [11] Tetrahedron Letters, 2006, vol. 47, # 50, p. 8981 - 8982 [12] Organic Letters, 2012, vol. 14, # 8, p. 2138 - 2141 [13] Patent: , 2016, . Location in patent: Paragraph 0037 [14] Patent: CN108774252, 2018, A. Location in patent: Paragraph 0032; 0034