维他命D2二氧化硫加合物合成路线 （共 20 条）
反应条件
Multi-step reaction with 2 steps 1: imidazole / Ambient temperature2: 94 percent / NaHCO3 / aq. ethanol / 1.25 h / Heating
参考文献
Choudhry, Satish C.; Belica, Peter S.; Coffen, David L.; Focella, Antonino; Maehr, Hubert; et al. Journal of Organic Chemistry, 1993 , vol. 58, # 6 p. 1496 - 1500
反应条件
Multi-step reaction with 5 steps 1: 1H-imidazole / dichloromethane / 5 - 20 °C / |Inert atmosphere2: sodium acetate; acetic acid; ozone / methanol; dichloromethane / -25 °C / |Inert atmosphere3: sodium tetrahydroborate / methanol; dichloromethane / 2.5 h / -25 - 20 °C / |Inert atmosphere4: 1H-imidazole; triphenylphosphine; iodine / dichloromethane / -2 - 20 °C / |Inert atmosphere5: sodium hydrogencarbonate / ethanol / 2 h / |Inert atmosphere; |Reflux
参考文献
Coutts, Lisa D.; Geiss, William B.; Gregg, Brian T.; Helle, Mark A.; King, Chi-Hsin R.; Itov, Zinovy; Mateo, Mary E.; Meckler, Harold; Zettler, Mark W.; Knutson, Joyce C. Organic Process Research and Development, 2002 , vol. 6, # 3 p. 246 - 255
反应条件
Multi-step reaction with 3 steps 1: 1H-imidazole / dichloromethane / 5 - 20 °C / |Inert atmosphere2: sodium acetate; acetic acid; ozone / methanol; dichloromethane / -25 °C / |Inert atmosphere3: sodium tetrahydroborate / methanol; dichloromethane / 2.5 h / -25 - 20 °C / |Inert atmosphere
参考文献
Coutts, Lisa D.; Geiss, William B.; Gregg, Brian T.; Helle, Mark A.; King, Chi-Hsin R.; Itov, Zinovy; Mateo, Mary E.; Meckler, Harold; Zettler, Mark W.; Knutson, Joyce C. Organic Process Research and Development, 2002 , vol. 6, # 3 p. 246 - 255
反应条件
Multi-step reaction with 5 steps 1: 42 percent / imidazole / dimethylformamide / 1.5 h / 20 °C2: sodium hydrogen carbonate / aq. ethanol / 1.5 h / Heating3: N-methylmorpholine N-oxide monohydrate, selenium dioxide / CH2Cl2; methanol / 0.83 h / Heating4: imidazole / dimethylformamide / 1.5 h / 20 °C5: liq. SO2 / diethyl ether / 0.5 h / Heating
参考文献
Calverley Tetrahedron, 1987 , vol. 43, # 20 p. 4609-4619
反应条件
Multi-step reaction with 6 steps 1: imidazole / Ambient temperature2: 94 percent / NaHCO3 / aq. ethanol / 1.25 h / Heating3: 54.9 g / SeO2, 4-methylmorpholine N-oxide / methanol / 5.5 h / Heating4: imidazole / CH2Cl2 / 6 h / Ambient temperature5: 63.8 g / SO2 / CH2Cl2 / 0.75 h / -10 °C6: 1) O3, 2) Ph3P / 1) CH2Cl2, MeOH, -10 deg C, 40 min, 2) room temperature, 3 h
参考文献
Choudhry, Satish C.; Belica, Peter S.; Coffen, David L.; Focella, Antonino; Maehr, Hubert; et al. Journal of Organic Chemistry, 1993 , vol. 58, # 6 p. 1496 - 1500
反应条件
Multi-step reaction with 5 steps 1: 42 percent / imidazole / dimethylformamide / 1.5 h / 20 °C2: sodium hydrogen carbonate / aq. ethanol / 1.5 h / Heating3: N-methylmorpholine N-oxide monohydrate, selenium dioxide / CH2Cl2; methanol / 0.83 h / Heating4: imidazole / dimethylformamide / 1.5 h / 20 °C5: liq. SO2 / diethyl ether / 0.5 h / Heating
参考文献
Calverley Tetrahedron, 1987 , vol. 43, # 20 p. 4609-4619
反应条件
Multi-step reaction with 6 steps 1: imidazole / Ambient temperature2: 94 percent / NaHCO3 / aq. ethanol / 1.25 h / Heating3: 54.9 g / SeO2, 4-methylmorpholine N-oxide / methanol / 5.5 h / Heating4: imidazole / CH2Cl2 / 6 h / Ambient temperature5: 63.8 g / SO2 / CH2Cl2 / 0.75 h / -10 °C6: 1) O3, 2) Ph3P / 1) CH2Cl2, MeOH, -10 deg C, 40 min, 2) room temperature, 3 h
参考文献
Choudhry, Satish C.; Belica, Peter S.; Coffen, David L.; Focella, Antonino; Maehr, Hubert; et al. Journal of Organic Chemistry, 1993 , vol. 58, # 6 p. 1496 - 1500
反应条件
Multi-step reaction with 3 steps 1: 42 percent / imidazole / dimethylformamide / 1.5 h / 20 °C2: 1.) ozone 2.) PPh3 / 1.) CH2Cl2, MeOH, -60 deg C 2.) CH2Cl2, MeOH, -60 to 0 deg C3: NaHCO3 / aq. ethanol / Heating
参考文献
Calverley Tetrahedron, 1987 , vol. 43, # 20 p. 4609-4619
反应条件
Multi-step reaction with 4 steps 1: 42 percent / imidazole / dimethylformamide / 1.5 h / 20 °C2: 1.) ozone 2.) PPh3 / 1.) CH2Cl2, MeOH, -60 deg C 2.) CH2Cl2, MeOH, -60 to 0 deg C3: NaHCO3 / aq. ethanol / Heating
参考文献
Calverley Tetrahedron, 1987 , vol. 43, # 20 p. 4609-4619
反应条件
Multi-step reaction with 7 steps 1: 42 percent / imidazole / dimethylformamide / 1.5 h / 20 °C2: sodium hydrogen carbonate / aq. ethanol / 1.5 h / Heating3: N-methylmorpholine N-oxide monohydrate, selenium dioxide / CH2Cl2; methanol / 0.83 h / Heating4: imidazole / dimethylformamide / 1.5 h / 20 °C5: liq. SO2 / diethyl ether / 0.5 h / Heating6: 1.) ozone 2.) PPh3 / 1.) CH2Cl2, MeOH, -60 deg C, 40 min. 2.) CH2Cl2, MeOH, -60 to 0 deg C7: 5 percent / NaHCO3 / ethanol / 1.5 h / Heating
参考文献
Calverley Tetrahedron, 1987 , vol. 43, # 20 p. 4609-4619
