2-乙酰基氨基-3-(3-羟基-苯基)-丙酸甲酯合成路线 (共 6 条)
反应条件
1: Bacillus licheniformis protease; sodium hydroxide / aq. phosphate buffer / 9 h / 20 °C / pH 7.5 / |Resolution of racemate; |Enzymatic reaction 2: hydrogenchloride / aq. phosphate buffer / 2 h / 100 °C View Scheme
参考文献
Humphrey, Cara E.; Furegati, Markus; Laumen, Kurt; Vecchia, Luigi La; Leuten, Thomas; Constanze D Mueller-Hartwieg; Voegtle, Markus
Organic Process Research and Development, 2007 , vol. 11, # 6 p. 1069 - 1075
反应条件
1: Bacillus licheniformis protease; sodium hydroxide / aq. phosphate buffer / 9 h / 20 °C / pH 7.5 / |Resolution of racemate; |Enzymatic reaction 2: hydrogenchloride / aq. phosphate buffer / 2 h / 100 °C View Scheme
参考文献
Humphrey, Cara E.; Furegati, Markus; Laumen, Kurt; Vecchia, Luigi La; Leuten, Thomas; Constanze D Mueller-Hartwieg; Voegtle, Markus
Organic Process Research and Development, 2007 , vol. 11, # 6 p. 1069 - 1075
反应条件
hydrogen; palladium 10 on activated carbon in methanol; ethyl acetate
T=50°C; P=30003 Torr;
参考文献
AUSPEX PHARMACEUTICALS, INC.; GANT, Thomas, G.; HODILUK, Craig; WOO, Soon, H.
Patent: WO2010/54286 A2, 2010 ;
Location in patent: Page/Page column 40 ;
反应条件
1: acetic anhydride; sodium acetate / 3.5 h / 115 °C / |Inert atmosphere
2: hydrogen; palladium 10 on activated carbon / methanol / 4 h / 825.08 Torr
View Scheme
参考文献
Humphrey, Cara E.; Furegati, Markus; Laumen, Kurt; Vecchia, Luigi La; Leuten, Thomas; Constanze D Mueller-Hartwieg; Voegtle, Markus
Organic Process Research and Development, 2007 , vol. 11, # 6 p. 1069 - 1075
反应条件
1.1: acetic acid; pyridine / toluene / 24 h / 110 °C / |Reflux; |Inert atmosphere; |Dean-Stark; |Large scale
2.1: 5 palladium on charcoal; hydrogen / methanol / 4 h / 20 °C / 900.09 Torr / |Large scale
3.1: potassium carbonate / acetone; N,N-dimethyl-formamide / 20 h / 60 °C / |Reflux; |Large scale
4.1: sodium methylate / methanol / 10 - 40 °C / |Large scale
4.2: 2.5 h / 10 - 15 °C / |Large scale
5.1: zinc / acetic acid / 20 h / 40 - 45 °C / |Large scale
6.1: hydrogen; palladium 10 on activated carbon / methanol / 96 h / 20 °C / 900.09 Torr / |Large scale
View Scheme
参考文献
Humphrey, Cara E.; Furegati, Markus; Laumen, Kurt; Vecchia, Luigi La; Leuten, Thomas; Constanze D Mueller-Hartwieg; Voegtle, Markus
Organic Process Research and Development, 2007 , vol. 11, # 6 p. 1069 - 1075
反应条件
1.1: potassium carbonate / acetone; N,N-dimethyl-formamide / 20 h / 60 °C / |Reflux; |Large scale
2.1: sodium methylate / methanol / 10 - 40 °C / |Large scale
2.2: 2.5 h / 10 - 15 °C / |Large scale
3.1: zinc / acetic acid / 20 h / 40 - 45 °C / |Large scale
4.1: hydrogen; palladium 10 on activated carbon / methanol / 96 h / 20 °C / 900.09 Torr / |Large scale
View Scheme
参考文献
Humphrey, Cara E.; Furegati, Markus; Laumen, Kurt; Vecchia, Luigi La; Leuten, Thomas; Constanze D Mueller-Hartwieg; Voegtle, Markus
Organic Process Research and Development, 2007 , vol. 11, # 6 p. 1069 - 1075