5-(4-氨基-2-氧代-2H-嘧啶-1-基)-[1,3]1,3-氧硫杂环戊-2-甲酸孟酯合成路线 （共 18 条）
反应条件
1: 4-aminopyrimidin-2-one With N,O-bis-(trimethylsilyl)-acetamide in acetonitrile T=25 - 55°C; Inert atmosphere; 2: (1'R,2'S,5'R)-Menthyl 5(R)-acetoxy-1,3-oxathiolane-2(R)-carboxylate With zirconium tetrachloride in dichloromethane T=25 - 30°C; 6 h; Inert atmosphere; Reagent/catalystSolventConcentrationTime;
参考文献
LUPIN LIMITED; ROY, Bhairab, Nath; SINGH, Girij, Pal; SRIVASTAVA, Dhananjai; AHER, Umesh, Parasharam; PATIL, Sudhakar, Uttam
Patent: WO2013/21290 A1, 2013 ;
Location in patent: Page/Page column 19; 20 ;
反应条件
1: With methanesulfonic acid in ethanol; di-isopropyl ether T=20°C; 0.833333 h; 2: With triethylamine in hexane; water; ethyl acetate T=20°C; 1 h;
参考文献
WO2011/83484 A2, ;
Page/Page column 12-13 ;
反应条件
methanesulfonic acid in methanol T=25 - 30°C; 4.25 - 4.33333 h;
参考文献
WO2009/69011 A1, ;
Page/Page column 17 ;
反应条件
triethylamine in hexanes; ethanol; di-isopropyl ether; ethyl acetate T=20 - 30°C; Product distribution / selectivity;
参考文献
US2011/282046 A1, ;
Page/Page column 9 ;
反应条件
trimethylsilyl iodide in dichloromethane Vorbrueggen reaction;
参考文献
Goodyear, Michael D.; Hill, Malcolm L.; West, Jono P.; Whitehead, Andrew J.
Tetrahedron Letters, 2005 , vol. 46, # 49 p. 8535 - 8538
反应条件
1: SOCl2 / dimethylformamide; CH2Cl2 View Scheme
参考文献
Tetrahedron Letters, , vol. 46, # 49 p. 8535 - 8538
反应条件
1.1: N,N-dimethyl-formamide; methanesulfonic acid / dichloromethane / 8 - 12 °C 1.2: 2 h / 8 - 12 °C 2.1: triethylamine / dichloromethane / 8 - 50 °C 3.1: toluene / 1 h / Molecular sieve 4.1: toluene / 75 - 80 °C 5.1: methanesulfonic acid / methanol / 4 h 5.2: 0.17 h View Scheme
反应条件
1.1: 1,1,1,3,3,3-hexamethyl-disilazane / methanesulfonic acid / toluene / 4 h / Reflux 1.2: 15 - 57 °C 2.1: methanesulfonic acid / di-isopropyl ether; ethanol / 0.83 h / 20 °C 2.2: 1 h / 20 °C View Scheme
反应条件
trimethylsilyl iodide in dichloromethane 18 h; Yield given. Yields of byproduct given;
参考文献
Journal of Organic Chemistry, , vol. 60, # 8 p. 2621 - 2623
反应条件
1.1: toluene 1.2: 80 percent / Et3N / toluene; hexane 2.1: SOCl2 / dimethylformamide; CH2Cl2 View Scheme
参考文献
Tetrahedron Letters, , vol. 46, # 49 p. 8535 - 8538
