3-甲基-3,4-二氢-2H-1,4-苯并噁嗪合成路线 （共 12 条）
反应条件
hydrogen; sodium hydroxide; Amperkat SK Ni-Mo 3706 from HC Starck in methanol; toluene T=40°C; P=165017 Torr; pH=8 - 9; 1 h; Autoclave; Product distribution / selectivity;
参考文献
SALTIGO GMBH
Patent: US2011/40089 A1, 2011 ;
Location in patent: Page/Page column 5 ;
反应条件
1: in tetrahydrofuran T=5 - 50°C; 1.5 h; 2: With sodium tetrahydroborate; acetic acid in tetrahydrofuran T=5 - 20°C;
参考文献
F. HOFFMANN-LA ROCHE AG
Patent: WO2008/58867 A2, 2008 ;
Location in patent: Page/Page column 30-31 ;
WO 2008/058867 A2
反应条件
1.1: 90 percent / NaH / dimethylformamide / 6.5 h / 20 °C 2.1: O3 / methanol / -78 °C 2.2: Me2S; p-CH3C6H4SO3H / methanol / 4 h / -78 - 20 °C 2.3: 93 percent / amberlyst-15 / acetone / 12 h / 20 °C 3.1: 92 percent / H2 / Pd/C / methanol / 6 h / 25 °C / 3040 Torr View Scheme
参考文献
Journal of Heterocyclic Chemistry, , vol. 40, # 6 p. 1031 - 1039
反应条件
1.1: O3 / methanol / -78 °C 1.2: Me2S; p-CH3C6H4SO3H / methanol / 4 h / -78 - 20 °C 1.3: 93 percent / amberlyst-15 / acetone / 12 h / 20 °C 2.1: 92 percent / H2 / Pd/C / methanol / 6 h / 25 °C / 3040 Torr View Scheme
参考文献
Journal of Heterocyclic Chemistry, , vol. 40, # 6 p. 1031 - 1039
反应条件
aluminium trichloride in dichloromethane 46 h; Ambient temperature;
参考文献
Kawase; Kikugawa
Chemical and Pharmaceutical Bulletin, 1981 , vol. 29, # 6 p. 1615 - 1623
反应条件
1: 96 percent / pyridine-borane / ethanol / below 5 deg C 2: 31 percent / CF3COOH / 15 h / Heating View Scheme
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 29, # 6 p. 1615 - 1623
反应条件
1: 76 percent / pyridine-borane / ethanol / below 5 deg C 2: 31 percent / AlCl3(3eq.) / CH2Cl2 / 46 h / Ambient temperature View Scheme
参考文献
Chemical and Pharmaceutical Bulletin, , vol. 29, # 6 p. 1615 - 1623
反应条件
trifluoroacetic acid 15 h; Heating;
参考文献
Kawase; Kikugawa
Chemical and Pharmaceutical Bulletin, 1981 , vol. 29, # 6 p. 1615 - 1623
参考文献
Chemische Berichte, , vol. 30, p. 1635
反应条件
phosphoric acid; sodium hydroxide in water; toluene T=40 - 80°C; pH=2 - 3; 2.5 h; Industry scale;
参考文献
SALTIGO GMBH
Patent: US2010/222578 A1, 2010 ;
Location in patent: Page/Page column 5 ;
