[2-[(5-氯-苯并恶唑-2-基)(3-氧代丁基)氨基]乙基]氨基甲酸叔丁酯合成路线 （共 4 条）
反应条件
1.1: tetrahydrofuran / 5 - 60 °C 2.1: sodium acetate; sodium tris(acetoxy)borohydride; acetic acid / dichloromethane / 15 - 20 °C 3.1: tetrahydrofuran / 4.92 h / 20 °C / Resolution of racemate 3.2: 22.25 h / 20 °C / Resolution of racemate View Scheme
参考文献
MERCK SHARP and DOHME CORP.; MERCK SHARP and DOHME LIMITED; BAXTER, Carl, A.; CLEATOR, Edward; KRSKA, Shane, W.; SHEEN, Faye; STEWART, Gavin; STROTMAN, Neil; WALLACE, Debra, J.; WRIGHT, Timothy
Patent: WO2012/148553 A1, 2012 ;
WO 2012/148553 A1
反应条件
1: tetrahydrofuran / 5 - 60 °C 2: sodium acetate; sodium tris(acetoxy)borohydride; acetic acid / dichloromethane / 15 - 20 °C View Scheme
参考文献
MERCK SHARP and DOHME CORP.; MERCK SHARP and DOHME LIMITED; BAXTER, Carl, A.; CLEATOR, Edward; KRSKA, Shane, W.; SHEEN, Faye; STEWART, Gavin; STROTMAN, Neil; WALLACE, Debra, J.; WRIGHT, Timothy
Patent: WO2012/148553 A1, 2012 ;
WO 2012/148553 A1
反应条件
1.1: hydrogenchloride; water / 10 h / 20 - 30 °C 1.2: 35 °C / pH > 10 1.3: 24 h / -5 °C / Inert atmosphere 2.1: oxalyl dichloride / N,N-dimethyl-formamide / dichloromethane / 1 h / 0 - 10 °C / Industry scale 2.2: 1 h / 15 °C View Scheme
参考文献
MERCK SHARP and DOHME CORP.; MERCK SHARP and DOHME LIMITED; BAXTER, Carl, A.; CLEATOR, Edward; KRSKA, Shane, W.; SHEEN, Faye; STEWART, Gavin; STROTMAN, Neil; WALLACE, Debra, J.; WRIGHT, Timothy
Patent: WO2012/148553 A1, 2012 ;
WO 2012/148553 A1
反应条件
1: With hydrogenchloride; water T=20 - 30°C; 10 h; 2: With potassium phosphate in toluene T=35°C; pH=> 10; 3: With formic acid; triethylamine; (CH3C6H4CH(CH3)2)RuCl(NH2CH(C6H5)CH(C6H5)NSO2C6H2(CH(CH3)2)3) in toluene; acetonitrile T=-5°C; 24 h; Inert atmosphere;
参考文献
MERCK SHARP and DOHME CORP.; MERCK SHARP and DOHME LIMITED; BAXTER, Carl, A.; CLEATOR, Edward; KRSKA, Shane, W.; SHEEN, Faye; STEWART, Gavin; STROTMAN, Neil; WALLACE, Debra, J.; WRIGHT, Timothy
Patent: WO2012/148553 A1, 2012 ;
Location in patent: Page/Page column 47-48 ;
WO 2012/148553 A1
