4,4-二甲氧基-3-甲基-2-丁烯酸乙酯合成路线 (共 10 条)
反应条件
hydrogenchloride; iodine 3 h; Heating;
参考文献
Yamano, Yumiko; Fujita, Yumi; Mizuguchi, Yukari; Nakagawa, Kimie; Okano, Toshio; Ito, Masayoshi; Wada, Akimori
Chemical and Pharmaceutical Bulletin, 2007 , vol. 55, # 9 p. 1365 - 1370
反应条件
1: With hydrazine T=20 - 60°C; 4 h; 2: With hydrogenchloride; water T=60°C; 5 h;
参考文献
AstraZeneca AB
Patent: US2009/111821 A1, 2009 ;
Location in patent: Page/Page column 23-24 ;
US 20090111821 A1
反应条件
1: 4.5 M H2SO4 / diethyl ether / 24 h / Ambient temperature 2: 1.) ethylmagnesium bromide / 1.) THF, room temperature, 1 h, 2.) THF, 15 min 3: DIBAH / tetrahydrofuran; toluene / 0.5 h / -78 °C 4: 95 percent / imidazole / dimethylformamide / 18 h / Ambient temperature 5: H2 / Lindlar catalyst / methanol / 24 h 6: LiAlH4, TiCl3 / tetrahydrofuran / 1 h / Ambient temperature 7: 80 percent / tetrabutylammonium fluoride / tetrahydrofuran / 2 h / Ambient temperature View Scheme
参考文献
Solladie, Guy; Girardin, Andre
Tetrahedron Letters, 1988 , vol. 29, # 2 p. 213 - 216
反应条件
1: 4.5 M H2SO4 / diethyl ether / 24 h / Ambient temperature 2: 1.) ethylmagnesium bromide / 1.) THF, room temperature, 1 h, 2.) THF, 15 min 3: DIBAH / tetrahydrofuran; toluene / 0.5 h / -78 °C 4: 95 percent / imidazole / dimethylformamide / 18 h / Ambient temperature 5: H2 / Lindlar catalyst / methanol / 24 h 6: LiAlH4, TiCl3 / tetrahydrofuran / 1 h / Ambient temperature 7: 80 percent / tetrabutylammonium fluoride / tetrahydrofuran / 2 h / Ambient temperature 8: MnO2 / CH2Cl2 / 2 h / Ambient temperature 9: 80 percent / AgO, NaCN / methanol / 18 h / Ambient temperature View Scheme
参考文献
Solladie, Guy; Girardin, Andre
Tetrahedron Letters, 1988 , vol. 29, # 2 p. 213 - 216
反应条件
1: 4.5 M H2SO4 / diethyl ether / 24 h / Ambient temperature 2: 1.) ethylmagnesium bromide / 1.) THF, room temperature, 1 h, 2.) THF, 15 min 3: DIBAH / tetrahydrofuran; toluene / 0.5 h / -78 °C 4: 95 percent / imidazole / dimethylformamide / 18 h / Ambient temperature 5: H2 / Lindlar catalyst / methanol / 24 h 6: LiAlH4, TiCl3 / tetrahydrofuran / 1 h / Ambient temperature 7: 80 percent / tetrabutylammonium fluoride / tetrahydrofuran / 2 h / Ambient temperature 8: MnO2 / CH2Cl2 / 2 h / Ambient temperature View Scheme
参考文献
Solladie, Guy; Girardin, Andre
Tetrahedron Letters, 1988 , vol. 29, # 2 p. 213 - 216
反应条件
hydrogenchloride in dichloromethane 1.5 h;
参考文献
Curley, Robert W.; Ticoras, Christ J.
Synthetic Communications, 1986 , vol. 16, # 6 p. 627 - 632
反应条件
lithium aluminium tetrahydride in tetrahydrofuran
T=0°C; 1 h; Yield given. Yields of byproduct given. Title compound not separated from byproducts;
参考文献
Ferraboschi, Patrizia; Grisenti, Paride; Casati, Rosangela; Fiecchi, Alberto; Santaniello, Enzo
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1987 , p. 1743 - 1748
反应条件
Saccharomyces cerevisiae; [14C]-Sucrose in water
T=30°C; 96 h;
参考文献
Ferraboschi, Patrizia; Grisenti, Paride; Casati, Rosangela; Fiecchi, Alberto; Santaniello, Enzo
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1987 , p. 1743 - 1748
反应条件
1: 53 percent / 1 M HCl / dioxane / 4 h / Ambient temperature
2: 60 percent / NH4Cl / methanol / 0.5 h / Heating
3: 40 percent / Saccharomyces cerevisiae, saccharose / H2O / 144 h / 30 °C
View Scheme
参考文献
Ferraboschi, Patrizia; Grisenti, Paride; Casati, Rosangela; Fiecchi, Alberto; Santaniello, Enzo
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1987 , p. 1743 - 1748
反应条件
1: 7.1 g / aq. HCl / CH2Cl2 / 2 h / 0 °C
2: chiral oxazaborolidinium salt / CH2Cl2 / 8 h / -78 °C
3: diethyl ether; tetrahydrofuran / 1 h / -40 °C
4: LiAlH4 / diethyl ether / 2 h / 0 °C
5: 46.5 mg / DMSO; oxalyl chloride; Et3N / CH2Cl2 / -78 - 20 °C
6: KOH / methanol / 0.5 h / Heating
7: 7.5 mg / aq. HCl; AcOH / 3 h / 20 °C
View Scheme
参考文献
Hu, Qi-Ying; Rege, Pankaj D.; Corey
Journal of the American Chemical Society, 2004 , vol. 126, # 19 p. 5984 - 5986