1: methyl-magnesium chloride With anhydrous iron chloride; lithium chloride in tetrahydrofuran T=-35°C; 2: 5-alpha-pregnane-3,20-dione in tetrahydrofuran T=-35 - -18°C; 3 h; 3: With hydrogenchloride; water in tetrahydrofuran T=25°C; Product distribution / selectivity;
参考文献
MARINUS PHARMACEUTICALS, INC.; SHAW, Kenneth; HUTCHISON, Alan
Patent: WO2011/19821 A2, 2011 ;
Location in patent: Page/Page column 12 ;
1: methyl-magnesium chloride With anhydrous iron chloride; lithium chloride in tetrahydrofuran T=-35 - -27°C; Inert atmosphere; 2: 5-alpha-pregnane-3,20-dione in tetrahydrofuran T=-25 - -20°C; Inert atmosphere; 3: With hydrogenchloride; water in tetrahydrofuran Product distribution / selectivity;
参考文献
MARINUS PHARMACEUTICALS, INC.; SHAW, Kenneth; HUTCHISON, Alan
Patent: WO2011/19821 A2, 2011 ;
Location in patent: Page/Page column 14 ;
1: methyl-magnesium chloride With titanium tetraethoxide; titanium tetrachloride in tetrahydrofuran T=5°C; 0.333333 h; 2: 5-alpha-pregnane-3,20-dione in tetrahydrofuran T=5 - 40°C; 4 h; 3: With hydrogenchloride; water in ethyl acetate Product distribution / selectivity;
参考文献
MARINUS PHARMACEUTICALS, INC.; SHAW, Kenneth; HUTCHISON, Alan
Patent: WO2011/19821 A2, 2011 ;
Location in patent: Page/Page column 11 ;
1: methyl-magnesium chloride With anhydrous iron chloride in tetrahydrofuran T=-40°C; 0.166667 h; 2: 5-alpha-pregnane-3,20-dione in tetrahydrofuran T=-40 - -20°C; 2.5 h; 3: With hydrogenchloride; water in tetrahydrofuran Product distribution / selectivity;
参考文献
MARINUS PHARMACEUTICALS, INC.; SHAW, Kenneth; HUTCHISON, Alan
Patent: WO2011/19821 A2, 2011 ;
Location in patent: Page/Page column 11-12 ;
Amato, Joseph S.; Chung, John Y. L.; Cvetovich, Raymond J.; Gong, Xiaoyi; McLaughlin, Mark; Reamer, Robert A.
Journal of Organic Chemistry, 2005 , vol. 70, # 5 p. 1930 - 1933
in not given Cl3Si(OC2H5), Si(OC2H5)4 and CH3MgCl; hydrolysis;;
参考文献
Rathousky, J.; Chvalovsky, V.; Bazant, V.
Chemicke Listy, 1953 , vol. 47, p. 1387 - 1393
C. A., 1955 , p. 161
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Gmelin Handbook: Si: MVol.C, 107, page 296 - 298
