6-(羟基甲基)-2H-吡啶并[3,2-b][1,4]噁嗪-3(4H)-酮合成路线 （共 7 条）
反应条件
palladium 10 on activated carbon; hydrogen in methanol; dichloromethane
T=20°C; P=750.075 Torr; 7 h;
参考文献
KYORIN PHARMACEUTICAL CO., LTD.; MERCK SHARP and DOHME CORP.; FUKUDA, Yasumichi; KAELIN, David E. Jr.; SINGH, Sheo B.
Patent: WO2013/3383 A1, 2013 ;
Location in patent: Page/Page column 89-90 ;
反应条件
1.1: sodium methylate / methanol / 0.5 h / 20 °C
1.2: 2 h / 0 °C
2.1: potassium carbonate / acetone / 8 h / |Reflux
3.1: acetic acid; iron / 1.5 h / 90 °C
4.1: tetrakis(triphenylphosphine) palladium(0); potassium carbonate / water; 1,4-dioxane / 24 h / |Reflux
5.1: ozone / dichloromethane; methanol / -71 °C
6.1: hydrogen; palladium 10 on activated carbon / dichloromethane; methanol / 7 h / 20 °C / 750.08 Torr
View Scheme
参考文献
KYORIN PHARMACEUTICAL CO., LTD.; MERCK SHARP and DOHME CORP.; FUKUDA, Yasumichi; KAELIN, David E. Jr.; SINGH, Sheo B.
Patent: WO2013/3383 A1, 2013 ;
反应条件
1: potassium carbonate / acetone / 8 h / |Reflux
2: acetic acid; iron / 1.5 h / 90 °C
3: tetrakis(triphenylphosphine) palladium(0); potassium carbonate / water; 1,4-dioxane / 24 h / |Reflux
4: ozone / dichloromethane; methanol / -71 °C
5: hydrogen; palladium 10 on activated carbon / dichloromethane; methanol / 7 h / 20 °C / 750.08 Torr
View Scheme
参考文献
KYORIN PHARMACEUTICAL CO., LTD.; MERCK SHARP and DOHME CORP.; FUKUDA, Yasumichi; KAELIN, David E. Jr.; SINGH, Sheo B.
Patent: WO2013/3383 A1, 2013 ;
反应条件
1: acetic acid; iron / 1.5 h / 90 °C
2: tetrakis(triphenylphosphine) palladium(0); potassium carbonate / water; 1,4-dioxane / 24 h / |Reflux
3: ozone / dichloromethane; methanol / -71 °C
4: hydrogen; palladium 10 on activated carbon / dichloromethane; methanol / 7 h / 20 °C / 750.08 Torr
View Scheme
参考文献
KYORIN PHARMACEUTICAL CO., LTD.; MERCK SHARP and DOHME CORP.; FUKUDA, Yasumichi; KAELIN, David E. Jr.; SINGH, Sheo B.
Patent: WO2013/3383 A1, 2013 ;
反应条件
1: tetrakis(triphenylphosphine) palladium(0); potassium carbonate / water; 1,4-dioxane / 24 h / |Reflux
2: ozone / dichloromethane; methanol / -71 °C
3: hydrogen; palladium 10 on activated carbon / dichloromethane; methanol / 7 h / 20 °C / 750.08 Torr
View Scheme
参考文献
KYORIN PHARMACEUTICAL CO., LTD.; MERCK SHARP and DOHME CORP.; FUKUDA, Yasumichi; KAELIN, David E. Jr.; SINGH, Sheo B.
Patent: WO2013/3383 A1, 2013 ;
反应条件
1: ozone / dichloromethane; methanol / -71 °C
2: hydrogen; palladium 10 on activated carbon / dichloromethane; methanol / 7 h / 20 °C / 750.08 Torr
View Scheme
参考文献
KYORIN PHARMACEUTICAL CO., LTD.; MERCK SHARP and DOHME CORP.; FUKUDA, Yasumichi; KAELIN, David E. Jr.; SINGH, Sheo B.
Patent: WO2013/3383 A1, 2013 ;
反应条件
manganese(IV) oxide in tetrahydrofuran; 1,4-dioxane; chloroform
T=40°C; 2 h;
参考文献
SMITHKLINE BEECHAM P.L.C.
Patent: WO2003/87098 A1, 2003 ;
Location in patent: Page/Page column 73 ;
