5-[双(2-氯乙基)氨基]-1-甲基-1H-苯并咪唑-2-丁酸甲酯合成路线 (共 12 条)
反应条件
hydrogenchloride 4 h; RefluxLarge scale reaction;
参考文献
Organic Process Research and Development, , vol. 15, # 5 p. 1063 - 1072
反应条件
1: in tetrahydrofuran
Inert atmosphereHeating;
2: With borane-THF in tetrahydrofuran
T=20°C;
3: With methanol in tetrahydrofuran
T=20°C;
参考文献
CEPHALON, INC.; CHEN, Jian; PRZYUSKI, Katrin; ROEMMELE, Renee, Caroline
Patent: WO2010/42568 A1, 2010 ;
Location in patent: Page/Page column 19-20 ;
反应条件
methanesulfonic acid
T=65°C; 1 h; Inert atmosphere;
参考文献
CEPHALON, INC.; BAKALE, Roger, P.; BROWN, Peter, D.; CHEN, Jian; DRAGER, Anthony, S.; LABELL, Rachel, Y.; MCKEAN, Robert, E.; PATEL, Piyush, R.; ROEMMELE, Renee, C.
Patent: WO2014/75035 A1, 2014 ;
Location in patent: Page/Page column 15 ;
反应条件
borane-THF in tetrahydrofuran
T=20 - 58°C; 2.66667 h; Inert atmosphere;
参考文献
CEPHALON, INC.; BAKALE, Roger, P.; BROWN, Peter, D.; CHEN, Jian; DRAGER, Anthony, S.; LABELL, Rachel, Y.; MCKEAN, Robert, E.; PATEL, Piyush, R.; ROEMMELE, Renee, C.
Patent: WO2014/75035 A1, 2014 ;
Location in patent: Page/Page column 15 ;
反应条件
trichlorophosphate
0.25 h; Reflux;
参考文献
Arevipharma GmbH; Schickaneder, Helmut; Schickaneder, Christian; Limmert, Michael
Patent: US2013/184471 A1, 2013 ;
Location in patent: Paragraph 0146; 0147; 0148; 0149; 0150 ;
反应条件
1: potassium carbonate / acetonitrile / 23 - 25 °C
2: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2068.65 Torr / Large scale reaction
3: sodium tetrahydroborate / 1,2-dichloro-ethane / 30 - 50 °C / Large scale reaction
View Scheme
参考文献
Chen, Jian; Przyuski, Katrin; Roemmele, Renee; Bakale, Roger P.
Organic Process Research and Development, 2011 , vol. 15, # 5 p. 1063 - 1072
反应条件
1: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2068.65 Torr / Large scale reaction
2: sodium tetrahydroborate / 1,2-dichloro-ethane / 30 - 50 °C / Large scale reaction
View Scheme
参考文献
Chen, Jian; Przyuski, Katrin; Roemmele, Renee; Bakale, Roger P.
Organic Process Research and Development, 2011 , vol. 15, # 5 p. 1063 - 1072
反应条件
1: toluene / 6 h / 95 - 105 °C / Large scale reaction
2: potassium carbonate / acetonitrile / 23 - 25 °C
3: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2068.65 Torr / Large scale reaction
4: sodium tetrahydroborate / 1,2-dichloro-ethane / 30 - 50 °C / Large scale reaction
View Scheme
参考文献
Chen, Jian; Przyuski, Katrin; Roemmele, Renee; Bakale, Roger P.
Organic Process Research and Development, 2011 , vol. 15, # 5 p. 1063 - 1072
反应条件
1: toluene / 6 h / 95 - 105 °C / Large scale reaction
2: potassium carbonate / acetonitrile / 23 - 25 °C
3: palladium 10 on activated carbon; hydrogen / methanol / 20 °C / 2068.65 Torr / Large scale reaction
4: sodium tetrahydroborate / 1,2-dichloro-ethane / 30 - 50 °C / Large scale reaction
View Scheme
参考文献
Chen, Jian; Przyuski, Katrin; Roemmele, Renee; Bakale, Roger P.
Organic Process Research and Development, 2011 , vol. 15, # 5 p. 1063 - 1072
反应条件
sodium tetrahydroborate in 1,2-dichloro-ethane
T=30 - 50°C; Large scale reaction;
参考文献
Chen, Jian; Przyuski, Katrin; Roemmele, Renee; Bakale, Roger P.
Organic Process Research and Development, 2011 , vol. 15, # 5 p. 1063 - 1072