4-[[(7R)-8-环戊基-7-乙基-5,6,7,8-四氢-5-甲基-6-氧代-2-喋啶基]氨基]-3-甲氧基-N-(1-甲基-4-哌啶基)苯甲酰胺合成路线 （共 7 条）
反应条件
1: (R)-4-(8-cyclopentyl-7-ethyl-5-methyl-6-oxo-5,6,7,8-tetrahydropteridin-2-ylamino)-3-methoxybenzoic acid With O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate; N-ethyl-N,N-diisopropylamine in dichloromethane T=25°C; 0.5 h; 2: 1-methyl-piperidin-4-ylamine in dichloromethane T=25°C; 2.5 h;
参考文献
US2006/35903 A1, ;
Page/Page column 21 ;
反应条件
toluene-4-sulfonic acid in methyl-isobutyl-carbinol 5 h; Heating / reflux;
参考文献
US2008/177066 A1, ;
Page/Page column 57; 60 ;
反应条件
1: (R)-4-(8-cyclopentyl-7-ethyl-5-methyl-6-oxo-5,6,7,8-tetrahydropteridin-2-ylamino)-3-methoxybenzoic acid With O-(1H-benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate; diisopropylamine in N,N-dimethyl-formamide T=20°C; 0.5 h; Inert atmosphere; 2: 1-methyl-piperidin-4-ylamine in N,N-dimethyl-formamide T=20°C; 3 h; Inert atmosphere;
参考文献
Budin, Ghyslain; Yang, Katherine S.; Reiner, Thomas; Weissleder, Ralph
Angewandte Chemie - International Edition, 2011 , vol. 50, # 40 p. 9378 - 9381
反应条件
1.1: iron / acetic acid / 2.5 h / 70 - 100 °C / Inert atmosphere 2.1: sodium hydride / isobutyramide; mineral oil / -10 - 20 °C / Inert atmosphere 3.1: hydrogenchloride / ethanol; water / 48 h / Inert atmosphere; Reflux 4.1: O-(1H-benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate; diisopropylamine / N,N-dimethyl-formamide / 0.5 h / 20 °C / Inert atmosphere 4.2: 3 h / 20 °C / Inert atmosphere View Scheme
参考文献
Angewandte Chemie - International Edition, , vol. 50, # 40 p. 9378 - 9381
反应条件
1.1: sodium hydride / isobutyramide; mineral oil / -10 - 20 °C / Inert atmosphere 2.1: hydrogenchloride / ethanol; water / 48 h / Inert atmosphere; Reflux 3.1: O-(1H-benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate; diisopropylamine / N,N-dimethyl-formamide / 0.5 h / 20 °C / Inert atmosphere 3.2: 3 h / 20 °C / Inert atmosphere View Scheme
参考文献
Angewandte Chemie - International Edition, , vol. 50, # 40 p. 9378 - 9381
反应条件
1.1: hydrogenchloride / ethanol; water / 48 h / Inert atmosphere; Reflux 2.1: O-(1H-benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate; diisopropylamine / N,N-dimethyl-formamide / 0.5 h / 20 °C / Inert atmosphere 2.2: 3 h / 20 °C / Inert atmosphere View Scheme
参考文献
Angewandte Chemie - International Edition, , vol. 50, # 40 p. 9378 - 9381
反应条件
1.1: potassium carbonate / acetone / 0 - 20 °C / Inert atmosphere 2.1: iron / acetic acid / 2.5 h / 70 - 100 °C / Inert atmosphere 3.1: sodium hydride / isobutyramide; mineral oil / -10 - 20 °C / Inert atmosphere 4.1: hydrogenchloride / ethanol; water / 48 h / Inert atmosphere; Reflux 5.1: O-(1H-benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate; diisopropylamine / N,N-dimethyl-formamide / 0.5 h / 20 °C / Inert atmosphere 5.2: 3 h / 20 °C / Inert atmosphere View Scheme
参考文献
Angewandte Chemie - International Edition, , vol. 50, # 40 p. 9378 - 9381
