化学合成。
化学合成
合成路线 1(1. 合成:82962-54-7)
产率:78%
合成条件:With water; sodium chloride In dimethyl sulfoxide for 20 h; Reflux
实验步骤:2,2-二甲基-1,3-二恶烷-5,5-二羧酸酯S2(385g,1.5mol),NaCl(105g,1.8mol),水(58g,3.2mol)和二甲基亚砜(1500mL)的混合物 )回流20小时。 将溶液冷却至室温,加入饱和NaCl溶液(750mL),用乙醚(4×600mL)萃取产物。 用盐水(2×150mL)洗涤合并的有机萃取物,用Na 2 SO 4干燥。 蒸发溶剂,蒸馏残余油,得到3(220g,78%),为无色液体.1H NMR(700MHz,CDCl3,300K):δ= 4.16(q,J = 7.3Hz,2H),4.01- 4.08(m,4H),2.77-2.81(m,1H),1.43(s,3H),1.40(s,3H),1.26(t,J = 7.3Hz,3H)。
参考文献:
- [1] Synlett, 2017, vol. 28, # 5, p. 583 - 588 [2] Chemical and Pharmaceutical Bulletin, 1993, vol. 41, # 2, p. 339 - 345 [3] Journal of the American Chemical Society, 1987, vol. 109, # 26, p. 8071 - 8081 [4] Journal of Organic Chemistry, 1986, vol. 51, # 14, p. 2637 - 2641 [5] Patent: WO2012/103279, 2012, A2. Location in patent: Page/Page column 16-17 [6] Collection of Czechoslovak Chemical Communications, 2007, vol. 72, # 7, p. 965 - 983 [7] Angewandte Chemie - International Edition, 2018, vol. 57, # 2, p. 574 - 578 [8] Angew. Chem., 2018, vol. 130, p. 583 - 587,5 [9] Patent: WO2013/170030, 2013, A1. Location in patent: Page/Page column 56 [10] Patent: US2008/21032, 2008, A1. Location in patent: Page/Page column 81 [11] Patent: US4336408, 1982, A [12] Bioorganic and Medicinal Chemistry Letters, 2010, vol. 20, # 24, p. 7358 - 7360 [13] Organic Process Research and Development, 2012, vol. 16, # 9, p. 1527 - 1537