(8R,9S)-5-氟-8-(4-氟苯基)-2,7,8,9-四氢-9-(1-甲基-1H-1,2,4-三唑-5-基)-3H-吡啶并[4,3,2-de]酞嗪-3-酮合成路线 （共 19 条）
反应条件
CHIRALPAK IA in methanol; diethylamine Resolution of racemate;
参考文献
WO2013/28495 A1, ;
Paragraph 00394 ;
反应条件
1: acetic anhydride; triethylamine / dichloromethane; 2-methyl tetrahydrofuran / 20 - 95 °C / Industry scale 2: hydrogenchloride / methanol / 25 h / 20 °C 3: hydrogenchloride; titanium(III) chloride / water; tetrahydrofuran; methanol 4: hydrazine hydrate / methanol / 20 °C 5: CHIRALPAK IA column / diethylamine; carbon dioxide; methanol / Resolution of racemate View Scheme
反应条件
1: hydrogenchloride / methanol / 25 h / 20 °C 2: hydrogenchloride; titanium(III) chloride / water; tetrahydrofuran; methanol 3: hydrazine hydrate / methanol / 20 °C 4: CHIRALPAK IA column / diethylamine; carbon dioxide; methanol / Resolution of racemate View Scheme
反应条件
1: hydrogen / palladium 10 on activated carbon / methanol / 0.5 h / 20 °C / 760.05 Torr 2: hydrogenchloride; iron / water; methanol / 3 h / Reflux 3: hydrazine hydrate / methanol / 20 °C 4: CHIRALPAK IA column / diethylamine; carbon dioxide; methanol / Resolution of racemate View Scheme
反应条件
1: hydrogenchloride; titanium(III) chloride / tetrahydrofuran; methanol / 2 h / 30 - 50 °C 2: CHIRALPAK®IC / methanol / 35 °C 3: hydrazine hydrate / ethanol / 2 h / 20 °C View Scheme
反应条件
1: hydrogenchloride; titanium(III) chloride / tetrahydrofuran; methanol / 2 h / 30 - 50 °C 2: CHIRALPAK®IC / methanol / 35 °C 3: hydrazine hydrate / ethanol / 2 h / 20 °C View Scheme
反应条件
1: hydrogenchloride; iron / water; methanol / 24 h / |Reflux 2: CHIRALPAK®IC / methanol / 35 °C 3: hydrazine hydrate / ethanol / 2 h / 20 °C View Scheme
反应条件
1: hydrazine hydrate / methanol / 20 °C 2: CHIRALPAK IA / diethylamine; methanol / |Resolution of racemate View Scheme
反应条件
1: hydrogenchloride; iron / methanol / 3 h / |Reflux 2: CHIRALPAK®IC / methanol / 35 °C 3: hydrazine hydrate / ethanol / 2 h / 20 °C View Scheme
反应条件
1.1: 2-methyl tetrahydrofuran; triethylamine / dichloromethane / 0.17 h / |Large scale 1.2: 20 - 95 °C / |Large scale 2.1: hydrazine hydrate / tetrahydrofuran / 20 °C / |Inert atmosphere 2.2: 18 h / 60 °C 3.1: acetonitrile / 48 h / |Reflux; |Inert atmosphere 4.1: caesium carbonate / tetrahydrofuran / 4 h / 55 °C 5.1: CHIRALPAK IA / diethylamine; methanol / |Resolution of racemate View Scheme
