5,7-二氯吡啶并[4,3-d]嘧啶-4(3h)-酮合成路线 （共 8 条）
参考文献
Jang, Mi-Yeon; Jonghe, Steven De; Gao, Ling-Jie; Herdewijn, Piet
Tetrahedron Letters, 2006 , vol. 47, # 50 p. 8917 - 8920
反应条件
1.1: n-BuLi / diethyl ether / -78 - 20 °C
2.1: TFA / CH2Cl2 / 12 h / 20 °C
3.1: SOCl2 / 1,2-dichloro-ethane / 3 h / Heating
3.2: aq. NH3 / diethyl ether / 0.33 h / 0 °C
4.1: 3 h / Heating
View Scheme
参考文献
Jang, Mi-Yeon; Jonghe, Steven De; Gao, Ling-Jie; Herdewijn, Piet
Tetrahedron Letters, 2006 , vol. 47, # 50 p. 8917 - 8920
反应条件
1.1: TFA / CH2Cl2 / 12 h / 20 °C
2.1: SOCl2 / 1,2-dichloro-ethane / 3 h / Heating
2.2: aq. NH3 / diethyl ether / 0.33 h / 0 °C
3.1: 3 h / Heating
View Scheme
参考文献
Jang, Mi-Yeon; Jonghe, Steven De; Gao, Ling-Jie; Herdewijn, Piet
Tetrahedron Letters, 2006 , vol. 47, # 50 p. 8917 - 8920
反应条件
1.1: trichlorophosphate / 6 h / 160 - 165 °C / Sealed tube
2.1: N-ethyl-N,N-diisopropylamine; diphenyl phosphoryl azide / 6 h / Inert atmosphere; Reflux
3.1: N,N,N',N,-tetramethylethylenediamine; n-butyllithium / tetrahydrofuran / 2 h / -60 °C / Inert atmosphere
3.3: pH 2
4.1: 1,1'-carbonyldiimidazole / N,N-dimethyl-formamide / 2 h / 60 °C
4.2: 0 - 5 °C
5.1: 6 h / Inert atmosphere; Reflux
View Scheme
参考文献
ABBOTT LABORATORIES; ABBOTT LABORATORIES TRADING (SHANGHAI) COMPANY, LTD.; VASUDEVAN, Anil; PENNING, Thomas Dale; CHEN, Huanming; LIANG, Bo; WANG, Shaohui; ZHAO, Zhongqiang; CHAI, Dikun; YANG, Leifu; GAO, Yingxiang
Patent: WO2012/97682 A1, 2012 ;
反应条件
1.1: N-ethyl-N,N-diisopropylamine; diphenyl phosphoryl azide / 6 h / Inert atmosphere; Reflux
2.1: N,N,N',N,-tetramethylethylenediamine; n-butyllithium / tetrahydrofuran / 2 h / -60 °C / Inert atmosphere
2.3: pH 2
3.1: 1,1'-carbonyldiimidazole / N,N-dimethyl-formamide / 2 h / 60 °C
3.2: 0 - 5 °C
4.1: 6 h / Inert atmosphere; Reflux
View Scheme
参考文献
ABBOTT LABORATORIES; ABBOTT LABORATORIES TRADING (SHANGHAI) COMPANY, LTD.; VASUDEVAN, Anil; PENNING, Thomas Dale; CHEN, Huanming; LIANG, Bo; WANG, Shaohui; ZHAO, Zhongqiang; CHAI, Dikun; YANG, Leifu; GAO, Yingxiang
Patent: WO2012/97682 A1, 2012 ;
反应条件
1.1: SOCl2 / 1,2-dichloro-ethane / 3 h / Heating
1.2: aq. NH3 / diethyl ether / 0.33 h / 0 °C
2.1: 3 h / Heating
View Scheme
参考文献
Jang, Mi-Yeon; Jonghe, Steven De; Gao, Ling-Jie; Herdewijn, Piet
Tetrahedron Letters, 2006 , vol. 47, # 50 p. 8917 - 8920
反应条件
1.1: NaHDMS / tetrahydrofuran / 3 h / 29 °C
2.1: n-BuLi / diethyl ether / -78 - 20 °C
3.1: TFA / CH2Cl2 / 12 h / 20 °C
4.1: SOCl2 / 1,2-dichloro-ethane / 3 h / Heating
4.2: aq. NH3 / diethyl ether / 0.33 h / 0 °C
5.1: 3 h / Heating
View Scheme
参考文献
Jang, Mi-Yeon; Jonghe, Steven De; Gao, Ling-Jie; Herdewijn, Piet
Tetrahedron Letters, 2006 , vol. 47, # 50 p. 8917 - 8920
反应条件
triethylamine in 1,4-dioxane
T=80°C; 24 h;
参考文献
Jang, Mi-Yeon; Jonghe, Steven De; Gao, Ling-Jie; Herdewijn, Piet
Tetrahedron Letters, 2006 , vol. 47, # 50 p. 8917 - 8920
