2-溴-6-氟-4-甲基苯胺合成路线 （共 4 条）
反应条件
N-bromosuccinmide in acetic acid T=15 - 20°C; 1.66667 h;
参考文献
GLAXO GROUP LIMITED
Patent: WO2007/36715 A2, 2007 ;
Location in patent: Page/Page column 54-55 ;
WO 2007/036715 A2
反应条件
1: 2-bromo-6-fluoro-4-methylaniline With hydrogenchloride; sodium acetate; copper(II) sulfate; sodium sulfite; sodium nitrite in water T=0°C; 2: formaldehyd With hydroxylamine hydrochloride; sodium acetate in water 3: With hydrogenchloride in water Reflux;
参考文献
Yamakawa, Naoki; Suemasu, Shintaro; Okamoto, Yoshinari; Tanaka, Ken-Ichiro; Ishihara, Tomoaki; Asano, Teita; Miyata, Keishi; Otsuka, Masami; Mizushima, Tohru
Journal of Medicinal Chemistry, 2012 , vol. 55, # 11 p. 5143 - 5150
反应条件
1: With N,N-dicyclohexylamine; bis(η3-allyl-μ-chloropalladium(II)); bis[2-(diphenylphosphino)phenyl] ether in n-heptane; toluene
T=70°C; P=1725.17 Torr; 17 h; Inert atmosphere;
2: With tetrabutyl ammonium fluoride in tetrahydrofuran; methanol; n-heptane; toluene
T=80 - 85°C;
参考文献
MERCK SHARP andamp; DOHME CORP.; CHUNG, John, Y., L.; ZHANG, Yanfeng; ARTINO, Laura; BAXTER, Jennifer; COTE, Aaron, S.; DESMOND, Donal; SCOTT, Jeremy; VAYNSHTEYN, Yekaterina
Patent: WO2010/80971 A1, 2010 ;
Location in patent: Page/Page column 18-19 ;
WO 2010/080971 A1
反应条件
1.1: N,N-dicyclohexylmethylamine / toluene / 2 h / |Inert atmosphere
1.2: 72 - 75 °C / |Inert atmosphere
2.1: trifluoroacetic acid / methanol; toluene; tetrahydrofuran / 5 h / 30 - 85 °C
View Scheme
参考文献
Chung, John Y. L.; Steinhuebel, Dietrich; Krska, Shane W.; Hartner, Fred W.; Cai, Chaoxian; Rosen, Jonathan; Mancheno, Danny E.; Pei, Tao; Dimichele, Lisa; Ball, Richard G.; Chen, Cheng-Yi; Tan, Lushi; Alorati, Antony D.; Brewer, Sarah E.; Scott, Jeremy P.
Organic Process Research and Development, 2012 , vol. 16, # 11 p. 1832 - 1845
