5-甲基-8-硝基-6-氧代-5,6-二氢-4H-苯并[f]咪唑并[1,5-a][1,4]二氮杂卓-3-羧酸乙酯合成路线 (共 8 条)
反应条件
1: 97 percent / H2 / Pd/C / tetrahydrofuran; ethanol / 2 h 2: BF3*Et2O; t-butyl nitrite / CH2Cl2 / -15 - 5 °C 3: 160 mg / 0.67 h / 130 °C View Scheme
参考文献
Broggini, Gianluigi; Orlandi, Marco; Turconi, Alberto; Zoni, Caterina
Organic Preparations and Procedures International, 2003 , vol. 35, # 6 p. 609 - 613
反应条件
1: 7-nitro-3,4-dihydro-4-methyl-2H-1,4-benzodiazepine-2,5-(1H)-dione With potassium tert-butylate in tetrahydrofuran; N,N-dimethyl-formamide
T=0°C; 0.5 h; Inert atmosphere;
2: With diethyl chlorophosphate in tetrahydrofuran; N,N-dimethyl-formamide
T=0°C; 0.5 h; Inert atmosphere;
3: isocyano-acetic acid ethyl ester With potassium tert-butylate in tetrahydrofuran; N,N-dimethyl-formamide
T=0 - 20°C; 2.5 h; Inert atmosphere;
参考文献
GE HEALTHCARE LIMITED; WOODCRAFT, John; JONES, Clare; GAETA, Alessandra; TRIGG, William; JONES, Paul; PLANT, Stuart
Patent: WO2011/42550 A1, 2011 ;
Location in patent: Page/Page column 31-32 ;
反应条件
sulfuric acid; nitric acid in ethyl acetate
参考文献
Hoffmann-La Roche Inc.
Patent: US4352815 A1, 1982 ;
反应条件
1: C15H14BrN3O6 With N-bromosuccinmide; dibenzoyl peroxide in benzene
T=20°C; 22 h; Irradiation;
2: methylamine With N-ethyl-N,N-diisopropylamine in methanol
3 h; Reflux;
参考文献
Donohue, Sean R.; Dannals, Robert F.
Tetrahedron Letters, 2009 , vol. 50, # 52 p. 7271 - 7273
反应条件
in N-methyl-acetamide; water; acetic acid
参考文献
Hoffmann-La Roche Inc.
Patent: US4352815 A1, 1982 ;
反应条件
1: sodium hydride; diethyl chlorophosphate / tetrahydrofuran; dimethylformamide / 0.5 h / 0 °C
2: 1.79 g / sodium hydride / dimethylformamide; tetrahydrofuran / 18 h
View Scheme
参考文献
Broggini, Gianluigi; Orlandi, Marco; Turconi, Alberto; Zoni, Caterina
Organic Preparations and Procedures International, 2003 , vol. 35, # 6 p. 609 - 613
反应条件
1.1: dimethyl sulfoxide / 2.5 h / 140 °C
2.1: potassium tert-butylate / N,N-dimethyl-formamide; tetrahydrofuran / 0.5 h / 0 °C / Inert atmosphere
2.2: 0.5 h / 0 °C / Inert atmosphere
2.3: 2.5 h / 0 - 20 °C / Inert atmosphere
View Scheme
参考文献
GE HEALTHCARE LIMITED; WOODCRAFT, John; JONES, Clare; GAETA, Alessandra; TRIGG, William; JONES, Paul; PLANT, Stuart; JACKSON, Alexander
Patent: WO2011/42529 A1, 2011 ;
Title/Abstract Full Text Show Details
GE HEALTHCARE LIMITED; WOODCRAFT, John; JONES, Clare; GAETA, Alessandra; TRIGG, William; JONES, Paul; PLANT, Stuart
Patent: WO2011/42550 A1, 2011 ;
反应条件
sodium hydride in tetrahydrofuran; N,N-dimethyl-formamide
18 h;
参考文献
Broggini, Gianluigi; Orlandi, Marco; Turconi, Alberto; Zoni, Caterina
Organic Preparations and Procedures International, 2003 , vol. 35, # 6 p. 609 - 613