3-二乙氧基丙烷-1,1-二甲酸二乙酯合成路线 (共 10 条)
反应条件
potassium tert-butylate in N,N-dimethyl-formamide
参考文献
Mediver AB
Patent: US6184376 B2, 2001 ;
反应条件
Hg; sodium ethanolate in N-methyl-acetamide; water
反应条件
ethanol T=130 - 140°C;
参考文献
Journal of the Chemical Society, , vol. 75, p. 13
参考文献
Journal of the Chemical Society, , vol. 127, p. 194
反应条件
1.1: 94 percent / LiAlH4 / diethyl ether / 18 h / 20 °C 2.1: 83 percent / Dowex 50WX8-H(1+) resin / ethanol / 2 h / Heating 3.1: 99 percent / NEt3 / CH2Cl2 / 3 h / 0 - 20 °C 4.1: 47 percent / HCl / H2O; dioxane / 18 h / 20 °C 5.1: 95 percent / NEt3; DMAP; 3 Angstroem molecular sieves / acetonitrile / 1 h / 20 °C 6.1: bis(trimethylsilyl)acetamide / 1-methyl-pyrrolidin-2-one / 80 °C 6.2: 70 percent / TMSOTf / 1-methyl-pyrrolidin-2-one / 24 h / 0 °C 7.1: 87 percent / aq. NaOH / 3 h / 20 °C 8.1: 10 percent / DIBAL-H / tetrahydrofuran / 48 h / 20 °C View Scheme
参考文献
Geen, Graham R.; Kincey, Peter M.; Spoors, P. Grant
Tetrahedron Letters, 2001 , vol. 42, # 9 p. 1781 - 1784
反应条件
1.1: 94 percent / LiAlH4 / diethyl ether / 18 h / 20 °C 2.1: 83 percent / Dowex 50WX8-H(1+) resin / ethanol / 2 h / Heating 3.1: 99 percent / NEt3 / CH2Cl2 / 3 h / 0 - 20 °C 4.1: 47 percent / HCl / H2O; dioxane / 18 h / 20 °C 5.1: 95 percent / NEt3; DMAP; 3 Angstroem molecular sieves / acetonitrile / 1 h / 20 °C 6.1: bis(trimethylsilyl)acetamide / dimethylformamide / 1.5 h / 20 °C 6.2: 81 percent / TMSOTf / dimethylformamide / 3 h / 0 - 5 °C 7.1: 42 percent / aq. NaOH / dioxane / 4 h / 20 °C 8.1: DIBAL-H / tetrahydrofuran / 24 h / 20 °C 9.1: NEt3; DMAP / CH2Cl2 / 2 h / Heating View Scheme
参考文献
Geen, Graham R.; Kincey, Peter M.; Spoors, P. Grant
Tetrahedron Letters, 2001 , vol. 42, # 9 p. 1781 - 1784
反应条件
lithium aluminium tetrahydride in diethyl ether T=20°C; 18 h;
参考文献
Tetrahedron Letters, , vol. 42, # 9 p. 1781 - 1784
反应条件
1.1: 94 percent / LiAlH4 / diethyl ether / 18 h / 20 °C 2.1: 83 percent / Dowex 50WX8-H(1+) resin / ethanol / 2 h / Heating 3.1: 99 percent / NEt3 / CH2Cl2 / 3 h / 0 - 20 °C 4.1: 47 percent / HCl / H2O; dioxane / 18 h / 20 °C 5.1: 95 percent / NEt3; DMAP; 3 Angstroem molecular sieves / acetonitrile / 1 h / 20 °C 6.1: bis(trimethylsilyl)acetamide / dimethylformamide / 1.5 h / 20 °C 6.2: 81 percent / TMSOTf / dimethylformamide / 3 h / 0 - 5 °C 7.1: 42 percent / aq. NaOH / dioxane / 4 h / 20 °C 8.1: DIBAL-H / tetrahydrofuran / 24 h / 20 °C 9.1: NEt3; DMAP / CH2Cl2 / 2 h / Heating 10.1: 81 percent / hydrogen; NEt3 / Pd/C / ethyl acetate / 4 h / 50 °C / 760 Torr View Scheme
参考文献
Tetrahedron Letters, , vol. 42, # 9 p. 1781 - 1784
反应条件
1.1: 94 percent / LiAlH4 / diethyl ether / 18 h / 20 °C 2.1: 83 percent / Dowex 50WX8-H(1+) resin / ethanol / 2 h / Heating 3.1: 99 percent / NEt3 / CH2Cl2 / 3 h / 0 - 20 °C 4.1: 47 percent / HCl / H2O; dioxane / 18 h / 20 °C 5.1: 95 percent / NEt3; DMAP; 3 Angstroem molecular sieves / acetonitrile / 1 h / 20 °C 6.1: bis(trimethylsilyl)acetamide / dimethylformamide / 1.5 h / 20 °C 6.2: 81 percent / TMSOTf / dimethylformamide / 3 h / 0 - 5 °C 7.1: 42 percent / aq. NaOH / dioxane / 4 h / 20 °C 8.1: DIBAL-H / tetrahydrofuran / 24 h / 20 °C View Scheme
参考文献
Tetrahedron Letters, , vol. 42, # 9 p. 1781 - 1784
反应条件
sodium chloride in water; N,N-dimethyl-formamide
72 h; Heating;
参考文献
Langlois; Yang; Soulier; Florac
Synthetic Communications, 1992 , vol. 22, # 21 p. 3115 - 3127