5-氯-2-(六氢-5-甲基-1H-1,4-二氮杂卓-1-基)苯并恶唑合成路线 （共 6 条）
反应条件
1: dichloromethane; N,N-dimethyl-formamide / 1.75 h / 20 - 25 °C 2: triethylamine / dichloromethane / 2.5 h / 0 - 20 °C 3: 1,8-diazabicyclo[5.4.0]undec-7-ene / dichloromethane; water; acetonitrile / 10.08 h / 20 - 40 °C 4: tetrahydrofuran / 5 - 60 °C 5: 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: methanol; water / 2 h / 0 - 20 °C 2: dichloromethane; N,N-dimethyl-formamide / 1.75 h / 20 - 25 °C 3: triethylamine / dichloromethane / 2.5 h / 0 - 20 °C 4: 1,8-diazabicyclo[5.4.0]undec-7-ene / dichloromethane; water; acetonitrile / 10.08 h / 20 - 40 °C 5: tetrahydrofuran / 5 - 60 °C 6: 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: 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: 1,8-diazabicyclo[5.4.0]undec-7-ene / dichloromethane; water; acetonitrile / 10.08 h / 20 - 40 °C 2: tetrahydrofuran / 5 - 60 °C 3: sodium acetate; sodium tris(acetoxy)borohydride; acetic acid / dichloromethane / 15 - 20 °C View Scheme
参考文献
Baxter, Carl A.; Cleator, Ed; Brands, Karel M. J.; Edwards, John S.; Reamer, Robert A.; Sheen, Faye J.; Stewart, Gavin W.; Strotman, Neil A.; Wallace, Debra J.
Organic Process Research and Development, 2011 , vol. 15, # 2 p. 367 - 375
反应条件
1: triethylamine / dichloromethane / 2.5 h / 0 - 20 °C 2: 1,8-diazabicyclo[5.4.0]undec-7-ene / dichloromethane; water; acetonitrile / 10.08 h / 20 - 40 °C 3: tetrahydrofuran / 5 - 60 °C 4: sodium acetate; sodium tris(acetoxy)borohydride; acetic acid / dichloromethane / 15 - 20 °C View Scheme
参考文献
Baxter, Carl A.; Cleator, Ed; Brands, Karel M. J.; Edwards, John S.; Reamer, Robert A.; Sheen, Faye J.; Stewart, Gavin W.; Strotman, Neil A.; Wallace, Debra J.
Organic Process Research and Development, 2011 , vol. 15, # 2 p. 367 - 375
反应条件
1: in tetrahydrofuran T=20°C; 4.91667 h; Resolution of racemate; 2: With isopropanol acetate in methanol T=20°C; 22.25 h; Resolution of racemate; optical yield given as percent ee;
参考文献
Baxter, Carl A.; Cleator, Ed; Brands, Karel M. J.; Edwards, John S.; Reamer, Robert A.; Sheen, Faye J.; Stewart, Gavin W.; Strotman, Neil A.; Wallace, Debra J.
Organic Process Research and Development, 2011 , vol. 15, # 2 p. 367 - 375
