N-[4-(4-氟苯基)-5-甲基-6-(1-甲基乙基)-2-嘧啶基]-N-甲基甲烷磺酰胺合成路线 (共 14 条)
反应条件
N-bromosuccinmide in acetonitrile 0.5 h; UV-irradiationInert atmosphereSealed flow reactor; Product distribution / selectivity;
参考文献
LEK PHARMACEUTICALS D.D.; CASAR, Zdenko; STERK, Damjan; JUKIC, Marko
Patent: WO2012/13325 A1, 2012 ;
Location in patent: Page/Page column 57-58 ;
反应条件
1: N-bromosuccinmide / acetonitrile / 0.5 h / UV-irradiation; Inert atmosphere; Sealed flow reactor 2: sodium hydrogencarbonate; water / acetonitrile / 4 h / Reflux View Scheme
参考文献
Sterk, Damjan; Casar, Zdenko; Jukic, Marko; Kosmrlj, Janez
Tetrahedron, 2012 , vol. 68, # 9 p. 2155 - 2160
反应条件
1: N-bromosuccinmide / acetonitrile / 16 h / 20 °C / Inert atmosphere; UV-irradiation 2: sodium hydrogencarbonate; dimethyl sulfoxide; sodium iodide / 71 h / 20 °C / Inert atmosphere View Scheme
参考文献
Sterk, Damjan; Casar, Zdenko; Jukic, Marko; Kosmrlj, Janez
Tetrahedron, 2012 , vol. 68, # 9 p. 2155 - 2160
反应条件
1: N-bromosuccinmide / acetonitrile / 0.5 h / UV-irradiation; Inert atmosphere; Sealed flow reactor 2: sodium hydrogencarbonate; water / acetonitrile / 4 h / Reflux 3: acetic anhydride; dimethyl sulfoxide / 85 °C View Scheme
反应条件
1: N-bromosuccinmide / acetonitrile / 16 h / 20 °C / Inert atmosphere; UV-irradiation 2: sodium hydrogencarbonate; dimethyl sulfoxide; sodium iodide / 71 h / 20 °C / Inert atmosphere View Scheme
参考文献
Tetrahedron, , vol. 68, # 9 p. 2155 - 2160
反应条件
triethylamine in dichloromethane
T=-5°C; 8 h; Inert atmosphere; Product distribution / selectivity;
参考文献
Sterk, Damjan; Casar, Zdenko; Jukic, Marko; Kosmrlj, Janez
Tetrahedron, 2012 , vol. 68, # 9 p. 2155 - 2160
反应条件
1: in tetrahydrofuran; water
T=-82 - -53°C;
2: With ammonium chloride in tetrahydrofuran; water
T=-53 - 20°C;
参考文献
LEK PHARMACEUTICALS D.D.; CASAR, Zdenko; KOSMRLJ, Janez
Patent: WO2010/86438 A1, 2010 ;
Location in patent: Page/Page column 24-25 ;
反应条件
(4R,6S)-4-(tert-butyldimethylsilyloxy)-6-(dihydroxymethyl)tetrahydro-2H-pyran-2-one in toluene
T=20°C; Wittig reaction;
参考文献
Casar, Zdenko; Steinbuecher, Miha; Kosmrlj, Janez
Journal of Organic Chemistry, 2010 , vol. 75, # 19 p. 6681 - 6684
反应条件
1: potassium carbonate / acetone / 24 h / 20 °C
2: caesium carbonate / 2-methyl tetrahydrofuran / 10 h / 40 °C
3: triethylamine / dichloromethane / 8 h / -5 °C / Inert atmosphere
View Scheme
参考文献
LEK PHARMACEUTICALS D.D.; CASAR, Zdenko; STERK, Damjan; JUKIC, Marko
Patent: WO2012/13325 A1, 2012 ;
反应条件
1: caesium carbonate / 2-methyl tetrahydrofuran / 10 h / 40 °C
2: triethylamine / dichloromethane / 8 h / -5 °C / Inert atmosphere
View Scheme
参考文献
LEK PHARMACEUTICALS D.D.; CASAR, Zdenko; STERK, Damjan; JUKIC, Marko
Patent: WO2012/13325 A1, 2012 ;