2,3-二甲基-4-甲氧基苯甲醛合成路线 （共 11 条）
参考文献
Dallacker,F.; Van Werst,J.
Chemische Berichte, 1972 , vol. 105, p. 2565 - 2574
反应条件
1: K2CO3 2: (i) POCl3, (ii) /BRN= 1859736/ View Scheme
参考文献
Dallacker,F.; Van Werst,J.
Chemische Berichte, 1972 , vol. 105, p. 2565 - 2574
反应条件
sodium chlorite; sodium dihydrogenphosphate in water; dimethyl sulfoxide T=20 - 40°C; 2 h;
参考文献
Merck Patent GmbH
Patent: US2011/60050 A1, 2011 ;
Location in patent: Page/Page column 4 ;
反应条件
1.1: sodium chlorite; sodium dihydrogenphosphate / water; dimethyl sulfoxide / 2 h / 20 - 40 °C 2.1: sec.-butyllithium / cyclohexane; tetrahydrofuran / 1 h / -78 °C / Inert atmosphere 2.2: 1 h / -78 °C 2.3: 0.5 h / 0 °C / pH 1 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 24 h / 0 - 20 °C 4.1: boron tribromide / dichloromethane / 3 h / 20 °C 5.1: Chiralpak AD column / isopropyl alcohol; n-heptane / Resolution of racemate View Scheme
参考文献
Merck Patent GmbH
Patent: US2011/60050 A1, 2011 ;
反应条件
1.1: sodium chlorite; sodium dihydrogenphosphate / water; dimethyl sulfoxide / 2 h / 20 - 40 °C
2.1: sec.-butyllithium / cyclohexane; tetrahydrofuran / 1 h / -78 °C / Inert atmosphere
2.2: 1 h / -78 °C
2.3: 0.5 h / 0 °C / pH 1
3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 24 h / 0 - 20 °C
4.1: boron tribromide / dichloromethane / 3 h / 20 °C
5.1: Chiralpak AD column / isopropyl alcohol; n-heptane / Resolution of racemate
View Scheme
参考文献
Merck Patent GmbH
Patent: US2011/60050 A1, 2011 ;
反应条件
potassium hydroxide; hydrazine hydrate; diethylene glycol
参考文献
Lejeune et al.
Bulletin de la Societe Chimique de France, 1957 , p. 1073,1076
反应条件
hydroxylamine-1-sulfonic acid in acetonitrile
T=60°C; 18 h;
参考文献
Chang, Chih-Shiang; Kan, Wai Ming; Chen, Chiu-Liang; Wang; Chern, Ji-Wang
Journal of the Chinese Chemical Society, 2002 , vol. 49, # 1 p. 83 - 89
反应条件
1: 96 percent / aq. hydroxylamine-sulfonic acid / acetonitrile / 18 h / 60 °C
2: 98 percent / BBr3 / CH2Cl2 / 6 h / 50 °C
View Scheme
参考文献
Chang, Chih-Shiang; Kan, Wai Ming; Chen, Chiu-Liang; Wang; Chern, Ji-Wang
Journal of the Chinese Chemical Society, 2002 , vol. 49, # 1 p. 83 - 89
反应条件
boron tribromide in dichloromethane
T=-78 - 20°C; 48 h;
参考文献
ACTELION PHARMACEUTICALS LTD
Patent: WO2005/2574 A1, 2005 ;
Location in patent: Page 48-49 ;
反应条件
1: 2.2 g / CrO3, HOAc / H2O / Ambient temperature
2: 1.15 g / BBr3 / CH2Cl2 / -70 - 20 °C
View Scheme
参考文献
Harris, Georgianna S.; Ellsworth, Kenneth; Witzel, Bruce E.; Tolman, Richard L.
Bioorganic Chemistry, 1996 , vol. 24, # 4 p. 386 - 400
