(4R,12aS)-3,4,6,8,12,12a-六氢-7-羟基-4-甲基-6,8-二氧代-2H-吡啶并[1',2':4,5]吡嗪并[2,1-b][1,3]恶嗪-9-羧酸合成路线 (共 2 条)
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1246616-73-8(4R,12aS)-3,4,6,8,12,12a-六氢-7-羟基-4-甲基-6,8-二氧代-2H-吡啶并[1',2':4,5]吡嗪并[2,1-b][1,3]恶嗪-9-羧酸
反应条件
Multi-step reaction with 6 steps 1.1: lithium hexamethyldisilazane / tetrahydrofuran / 2 h / -78 °C1.2: 0.33 h2.1: ethanol / 16 h / 0 - 20 °C3.1: N-bromosuccinmide / N,N-dimethyl-formamide / 48 h / 20 °C4.1: sulfuric acid / formic acid / 8 h / 20 °C5.1: acetic acid / toluene; methanol / 3 h / Reflux6.1: anhydrous potassium trimethylsilanolate / ethylene glycol dimethyl ether / 2 h / 20 - 60 °C
参考文献
Sumino, Yukihito; Okamoto, Kazuya; Masui, Moriyasu; Akiyama, Toshiyuki Patent: US2012/22251 A1, 2012 ;
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1246616-73-8(4R,12aS)-3,4,6,8,12,12a-六氢-7-羟基-4-甲基-6,8-二氧代-2H-吡啶并[1',2':4,5]吡嗪并[2,1-b][1,3]恶嗪-9-羧酸
反应条件
Multi-step reaction with 5 steps 1: ethanol / 16 h / 0 - 20 °C2: N-bromosuccinmide / N,N-dimethyl-formamide / 48 h / 20 °C3: sulfuric acid / formic acid / 8 h / 20 °C4: acetic acid / toluene; methanol / 3 h / Reflux5: anhydrous potassium trimethylsilanolate / ethylene glycol dimethyl ether / 2 h / 20 - 60 °C
参考文献
Sumino, Yukihito; Okamoto, Kazuya; Masui, Moriyasu; Akiyama, Toshiyuki Patent: US2012/22251 A1, 2012 ;