叔丁基二甲基甲硅烷基氧基乙酰氯合成路线 (共 5 条)
反应条件
oxalyl dichloride; N,N-dimethyl-formamide in dichloromethane
T=0°C; 3.5 h;
参考文献
Zeneca Limited
Patent: US6350775 B1, 2002 ;
Location in patent: Page column 29-30 ;
反应条件
thionyl chloride in dichloromethane
1.) reflux, 10 min, 2.) RT, 10 h;
参考文献
Mukaiyama, Teruaki; Shiina, Isamu; Uchiro, Hiromi; Kobayashi, Shu
Bulletin of the Chemical Society of Japan, 1994 , vol. 67, # 6 p. 1708 - 1716
反应条件
1: 97 percent / imidazole / dimethylformamide / 10 h / Ambient temperature
2: 71 percent / aq. K2CO3 / methanol; tetrahydrofuran / 1 h / Ambient temperature
3: 100 percent / thionyl chloride / CH2Cl2 / 1.) reflux, 10 min, 2.) RT, 10 h
View Scheme
参考文献
Mukaiyama, Teruaki; Shiina, Isamu; Uchiro, Hiromi; Kobayashi, Shu
Bulletin of the Chemical Society of Japan, 1994 , vol. 67, # 6 p. 1708 - 1716
反应条件
1: 90 percent / potassium hydroxide / tetrahydrofuran; methanol; H2O / 0.5 h / -10 - 5 °C
2: oxalyl chloride / benzene / 1.) RT, 30 min, 2.) reflux, 30 min
View Scheme
参考文献
Bischofberger, Norbert; Waldmann, Herbert; Saito, Tohru; Simon, Ethan S.; Lees, Watson; et al.
Journal of Organic Chemistry, 1988 , vol. 53, # 15 p. 3457 - 3465
反应条件
1.1: potassium hydroxide / ethanol / 12 h / 0 - 23 °C / Inert atmosphere
1.2: 0 °C / pH 4 / Inert atmosphere
2.1: oxalyl dichloride / benzene / 1 h / 23 - 90 °C / Inert atmosphere
View Scheme
参考文献
Vo, Cam-Van T.; Mitchell, T. Andrew; Bode, Jeffrey W.
Journal of the American Chemical Society, 2011 , vol. 133, # 35 p. 14082 - 14089