383-50-6 对甲苯磺酸氟乙酯

危险性质：非危险化学品

化学合成，医药氟罗沙星中间体；生化研究。

医药

合成路线 1（1. 合成：383-50-6）

产率：100% 合成条件：With 4-methyl-morpholine In dichloromethane at 20℃; for 17 h; 实验步骤：向反应容器中加入2-氟乙醇（1.00mL，16.9mmol），对甲苯磺酰氯（3.85g，20.2mmol），N-甲基吗啉（9.30mL，84.5mmol）和CH 2 Cl 2（50mL），进行反应。 在室温下保持17小时。 反应后，将水加入到反应体系中，用乙酸乙酯将产物萃取三次到有机层中。 用饱和盐水洗涤所得有机层并用MgSO 4干燥。 减压浓缩后，浓缩物经Hi-flash硅胶柱色谱纯化（展开溶剂，乙酸乙酯：己烷= 19：81→40：60），得到产物（3.79g（17.2mmol），产率> 100％， 淡黄色液体）。 114-NMR（600MHz，CDCl 3）：δ7.81（d，J = 8.4Hz，2H），7.36（d，J = 8.4Hz，2H），4.63-4.60（m，1H），4.55-4.52（m ，1H），4.31-4.27（m，1H），4.26-4.23（m，1H），2.46（s，3H）; 计算出的C 9 H 11 F 3 O（Mt）的LRMS（EI）：218.0，实测值：218.0。 参考文献：

• [1] Patent: US2018/30074, 2018, A1. Location in patent: Paragraph 0188-0191 [2] Journal of Labelled Compounds and Radiopharmaceuticals, 2008, vol. 51, # 7, p. 286 - 292 [3] Patent: US2013/177501, 2013, A1. Location in patent: Paragraph 0168 [4] Patent: US9168317, 2015, B2. Location in patent: Page/Page column 25; 26 [5] Patent: US9314541, 2016, B2. Location in patent: Page/Page column 26 [6] ChemMedChem, 2018, vol. 13, # 3, p. 241 - 250 [7] Tetrahedron, 2005, vol. 61, # 35, p. 8410 - 8418 [8] Journal of Organic Chemistry, 2004, vol. 69, # 18, p. 5934 - 5946 [9] Patent: US2009/110636, 2009, A1. Location in patent: Page/Page column 21-22 [10] ACS Medicinal Chemistry Letters, 2015, vol. 6, # 3, p. 260 - 265 [11] Patent: US2009/111990, 2009, A1. Location in patent: Page/Page column 21 [12] Synthesis, 1995, # 8, p. 989 - 997 [13] Molecular Pharmaceutics, 2015, vol. 12, # 7, p. 2265 - 2275 [14] ChemMedChem, 2016, vol. 11, # 1, p. 108 - 118 [15] Patent: WO2015/194954, 2015, A1. Location in patent: Page/Page column 9 [16] Journal of Medicinal Chemistry, 2014, vol. 57, # 2, p. 391 - 410 [17] Journal of Medicinal Chemistry, 2010, vol. 53, # 16, p. 6228 - 6239 [18] Bioorganic and Medicinal Chemistry Letters, 2015, vol. 25, # 2, p. 225 - 228 [19] Journal of Medicinal Chemistry, 2015, vol. 58, # 24, p. 9722 - 9730 [20] Chemical Communications, 2018, vol. 54, # 26, p. 3227 - 3230 [21] Bioorganic and Medicinal Chemistry, 2017, vol. 25, # 13, p. 3491 - 3499 [22] Journal of Medicinal Chemistry, 1980, vol. 23, # 9, p. 985 - 990 [23] Journal of Labelled Compounds and Radiopharmaceuticals, 2013, vol. 56, # 6, p. 313 - 316 [24] Journal of Labelled Compounds and Radiopharmaceuticals, 2014, vol. 57, # 5, p. 365 - 370 [25] Patent: JP5667058, 2015, B2. Location in patent: Paragraph 0705; 0706 [26] Journal of Medicinal Chemistry, 2016, vol. 59, # 20, p. 9422 - 9430 [27] Patent: US2015/197511, 2015, A1. Location in patent: Paragraph 0268; 0269 [28] Patent: EP2957556, 2015, A1. Location in patent: Paragraph 0056 [29] Patent: JP5851493, 2016, B2. Location in patent: Paragraph 0042 [30] Angewandte Chemie - International Edition, 2014, vol. 53, # 24, p. 6085 - 6089 [31] Angew. Chem., 2014, vol. 126, # 24, p. 6199 - 6203,5 [32] Patent: US2011/280808, 2011, A1. Location in patent: Page/Page column 73 [33] ChemMedChem, 2013, vol. 8, # 8, p. 1330 - 1344 [34] Journal of Medicinal Chemistry, 2012, vol. 55, # 5, p. 2342 - 2352 [35] Bioorganic and Medicinal Chemistry Letters, 2018, vol. 28, # 6, p. 1143 - 1148 [36] Journal of Chemical and Engineering Data, 1981, vol. 26, # 3, p. 344 - 346 [37] Journal of the American Chemical Society, 1987, vol. 109, # 13, p. 4036 - 4046 [38] Journal of Medicinal Chemistry, 2014, vol. 57, # 15, p. 6765 - 6780 [39] Bioorganic and medicinal chemistry letters, 2003, vol. 13, # 2, p. 201 - 204 [40] Patent: WO2013/48832, 2013, A1. Location in patent: Page/Page column 47 [41] Patent: WO2009/79683, 2009, A1. Location in patent: Page/Page column 43 [42] Journal of Medicinal Chemistry, 2013, vol. 56, # 17, p. 6858 - 6870 [43] Zhurnal Obshchei Khimii, 1949, vol. 19, p. 110 [44] Chem.Abstr., 1949, p. 6164 [45] Journal of the Chemical Society, 1948, p. 2175 [46] Journal of the American Chemical Society, 1955, vol. 77, p. 4899,4901 [47] Journal of the American Chemical Society, 1956, vol. 78, p. 3843,3845 [48] Journal of Medicinal Chemistry, 2007, vol. 50, # 23, p. 5752 - 5764 [49] ChemMedChem, 2010, vol. 5, # 5, p. 777 - 789 [50] Patent: EP2394668, 2011, A1 [51] Chemical Communications, 2012, vol. 48, # 7, p. 991 - 993 [52] Patent: EP2407455, 2012, A1. Location in patent: Page/Page column 11 [53] Organic and Biomolecular Chemistry, 2014, vol. 12, # 47, p. 9621 - 9630 [54] Organic and Biomolecular Chemistry, 2017, vol. 15, # 28, p. 5976 - 5982 [55] EJNMMI Research, 2017, vol. 7, [56] Molecules, 2018, vol. 23, # 5,