反应条件
1.1: zinc dibromide / dichloromethane / 1.5 h / 20 - 45 °C / Industry scale
2.1: sodium hydroxide; water / methanol / 16 h / 70 °C / Industry scale
2.2: 10 °C / pH ~ 1.5 / Industry scale
3.1: Oxonereg; / dichloromethane / 24 h / 15 °C / Industry scale
4.1: triethylamine; diphenyl phosphoryl azide / toluene / 9 h / 80 °C / 760.05 Torr / Industry scale; Reflux
5.1: triethylamine / toluene; water / 7 h / 0 - 20 °C / Industry scale
6.1: benzotriazol-1-ol; 4-methyl-morpholine; N'-(3-dimethylaminopropyl)-N-ethylcarbodiimide / acetonitrile; water / 5 h / 5 - 40 °C / Industry scale
7.1: sodium hydroxide; water / 2-methyl tetrahydrofuran / 7 h / 20 - 60 °C / Industry scale
7.2: 0.17 h / 20 - 30 °C / pH 1.5 - 3 / Industry scale
8.1: N-ethyl-N,N-diisopropylamine; benzotriazol-1-ol; N'-(3-dimethylaminopropyl)-N-ethylcarbodiimide / ethyl acetate; acetonitrile; water / -5 - 30 °C / Industry scale
9.1: sodium acetate; sodium hypochlorite; acetic acid; 2,2,6,6-tetramethyl-1-piperidinyloxy, free radical / methyl acetate; water; tert-butyl methyl ether / 2 h / 5 - 15 °C / Industry scale
View Scheme
参考文献
SCHERING CORPORATION; TRAVERSE, John; LEONG, William, W.; MILLER, Steven, P.; ALBANEZE-WALKER, Jennifer; HUNTER, Thomas, J.; WANG, Lijun; LIAO, Hongbiao; ARASAPPAN, Ashok; TRZASKA, Scott, T.; SMITH, Randi, M.; LEKHAL, Azzeddine; BOGEN, Stephane, L.; KONG, Jianshe; BENNETT, Frank; NJOROGE, F., George; POIRIER, Marc; KUO, Shen-Chun; CHEN, Yonggang; MATTHEWS, Kenneth S.; DEMONCHAUX, Patrice; FERREIRA, Amadeo
Patent: WO2011/14494 A1, 2011 ;