(8S,9R)-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 21 条）
反应条件
hydrazine hydrate in acetonitrile T=20°C; 2 h;
参考文献
BIOMARIN PHARMACEUTICAL INC.; FENG, Ying; GUTIERREZ, Andres, A.; SHEN, Yuqiao; WANG, Evelyn, W.; OKHAMAFE, Augustus, O.; PRICE, Christopher, P.; CHOU, Tianwei
Patent: WO2013/28495 A1, 2013 ;
Location in patent: Paragraph 00399 ;
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; TiCl3 / water; tetrahydrofuran; methanol / 2 h / 20 - 50 °C 2: methanol / 35 - 50 °C / Supercritical fluid chromtography using CHIRALPAK IC; Resolution of racemate 3: hydrazine hydrate / methanol / 10 h / 25 °C View Scheme
反应条件
1: hydrogenchloride; TiCl3 / water; tetrahydrofuran; methanol / 2 h / 20 - 50 °C 2: methanol / 35 - 50 °C / Supercritical fluid chromtography using CHIRALPAK IC; Resolution of racemate 3: hydrazine hydrate / methanol / 10 h / 25 °C View Scheme
反应条件
1: methanol / 35 - 50 °C / Supercritical fluid chromtography using CHIRALPAK IC; Resolution of racemate 2: hydrazine hydrate / methanol / 10 h / 25 °C View Scheme
反应条件
1: hydrogenchloride; iron / water; methanol / 24 h / |Reflux 2: hydrazine hydrate / methanol / 20 °C 3: CHIRALPAK IA / diethylamine; methanol / |Resolution of racemate View Scheme
反应条件
1: hydrogenchloride; iron / methanol / 3 h / |Reflux 2: hydrazine hydrate / methanol / 20 °C 3: CHIRALPAK IA / diethylamine; methanol / |Resolution of racemate View Scheme
