2-氧代-4-苯丁基磷酸二甲酯合成路线 (共 19 条)
反应条件
1: methanephosphonic acid dimethyl ester With n-butyllithium in tetrahydrofuran; hexane T=-78°C; 0.5 h; 2: methyl β-phenylpropionate in tetrahydrofuran; hexane T=-78 - 0°C;
参考文献
Kirsch, Stefan F.; Klahn, Philipp; Menz, Helge
Synthesis, 2011 , # 22 art. no. T78511SS, p. 3592 - 3603
反应条件
n-butyllithium 1.) THF, -78 deg C, 15 min, 2.) THF, -78 deg C, 30 min; Multistep reaction;
参考文献
May and Baker Limited
Patent: US4088695 A1, 1978 ;
反应条件
phosphorous acid trimethyl ester in acetonitrile
参考文献
Gutman, Arie; Nisnevich, Gennadiy; Etinger, Marina; Zaltzman, Igor; Judovich, Lev; Pertsikov, Boris
Patent: US2003/149294 A1, 2003 ;
反应条件
1.1: H2 / 5 percent Pd/C / ethyl acetate 2.1: MeOH 3.1: N-BuLi / tetrahydrofuran / 0 °C 3.2: tetrahydrofuran View Scheme
参考文献
DeLong, Mitchell A.; Amburgey, Jack; Taylor, Cynthia; Wos, John A.; Soper, David L.; Wang, Yili; Hicks, Renee
Bioorganic and Medicinal Chemistry Letters, 2000 , vol. 10, # 14 p. 1519 - 1522
反应条件
in acetonitrile T=20°C; 2.5 h; RefluxInert atmosphere;
参考文献
Harikrishna; Mohan, H. Rama; Dubey; Shankar; Subbaraju, Gottumukkala V.
Synthetic Communications, 2012 , vol. 42, # 9 p. 1288 - 1305
反应条件
1.1: MeOH 2.1: N-BuLi / tetrahydrofuran / 0 °C 2.2: tetrahydrofuran View Scheme
参考文献
DeLong, Mitchell A.; Amburgey, Jack; Taylor, Cynthia; Wos, John A.; Soper, David L.; Wang, Yili; Hicks, Renee
Bioorganic and Medicinal Chemistry Letters, 2000 , vol. 10, # 14 p. 1519 - 1522
反应条件
1: bromine / methanol / 2.83 h / -5 - 20 °C / Inert atmosphere 2: sodium iodide / acetone / 6 h / 20 °C / Inert atmosphere 3: acetonitrile / 2.5 h / 20 °C / Reflux; Inert atmosphere View Scheme
参考文献
Harikrishna; Mohan, H. Rama; Dubey; Shankar; Subbaraju, Gottumukkala V.
Synthetic Communications, 2012 , vol. 42, # 9 p. 1288 - 1305
反应条件
1: sodium iodide / acetone / 6 h / 20 °C / Inert atmosphere 2: acetonitrile / 2.5 h / 20 °C / Reflux; Inert atmosphere View Scheme
参考文献
Harikrishna; Mohan, H. Rama; Dubey; Shankar; Subbaraju, Gottumukkala V.
Synthetic Communications, 2012 , vol. 42, # 9 p. 1288 - 1305
反应条件
(i) NaH, THF, (ii) nBuLi, hexane, (iii) /BRN= 471308/; Multistep reaction;
参考文献
Grieco,P.A.; Pogonowski,C.S.
Journal of the American Chemical Society, 1973 , vol. 95, # 9 p. 3071 - 3072
反应条件
1.1: sodium hydride / tetrahydrofuran; mineral oil / 1 h / 0 - 20 °C / Inert atmosphere 1.2: 1.5 h / 0 °C 2.1: B-chloro-diisopinocampheylborane / n-heptane; tetrahydrofuran / 5 h / -30 - -25 °C / Inert atmosphere 2.2: 10 h / 20 °C 3.1: triethylamine; hydrogen / palladium 10 on activated carbon / tetrahydrofuran / 1 h / 20 °C / 760.05 Torr 4.1: 1H-imidazole / dichloromethane / 18 h / 20 °C 5.1: diisobutylaluminium hydride / dichloromethane; hexane / 0.5 h / -30 °C / Inert atmosphere 5.2: -30 °C 6.1: potassium tert-butylate / tetrahydrofuran / 0.5 h / 20 °C / Inert atmosphere 6.2: 3.25 h / 0 - 20 °C 7.1: hydrogenchloride / water; tetrahydrofuran / 18 h / 20 °C 7.2: pH 6.8 / Aqueous phosphate buffer View Scheme
参考文献
Biffi, Giancarlo; D'Alfonso, Alessandro; Feliciani, Lazzaro; Porta, Alessio; Vidari, Giovanni; Viscardi, Enrico; Zanoni, Giuseppe
Patent: US2012/16136 A1, 2012 ;