1-碘-3-甲氧基-2-(甲氧基甲氧基)苯合成路线 （共 6 条）
反应条件
1: With n-butyllithium in tetrahydrofuran T=-78°C; 2 h; 2: With iodine in tetrahydrofuran T=-50 - 20°C;
参考文献
MERCK SHARP and; DOHME CORP.; LIU, Kun; STACHEL, Shawn J.; COBURN, Craig A.; STEELE, Thomas G.; SOLL, Richard; WU, Hao; PENG, Xuanjin; CAI, Yaxian; DU, Xiaoxing; LI, Jian
Patent: WO2010/94242 A1, 2010 ;
Location in patent: Example 3.2 ;
WO 2010/094242 A1
反应条件
1.1: 99 percent / diisopropylethylamine / CH2Cl2 / 0 - 20 °C 2.1: n-butyllithium / tetrahydrofuran / 2 h / 20 °C 2.2: 30 percent / iodine / tetrahydrofuran / 2 h / 20 °C View Scheme
参考文献
Weeratunga, Gamini; Jaworska-Sobiesiak, Alina; Horne, Stephen; Rodrigo, Russel
Canadian Journal of Chemistry, 1987 , vol. 65, p. 2019 - 2023
反应条件
1: 80 percent / NaH / tetrahydrofuran 2: tBuLi / tetrahydrofuran View Scheme
参考文献
Tsang, Kit Y.; Brimble, Margaret A.; Bremner, John B.
Organic Letters, 2003 , vol. 5, # 23 p. 4425 - 4427
反应条件
hydrogenchloride in methanol T=0 - 20°C; 4 h;
参考文献
MERCK SHARP and; DOHME CORP.; LIU, Kun; STACHEL, Shawn J.; COBURN, Craig A.; STEELE, Thomas G.; SOLL, Richard; WU, Hao; PENG, Xuanjin; CAI, Yaxian; DU, Xiaoxing; LI, Jian
Patent: WO2010/94242 A1, 2010 ;
Location in patent: Example 3.3 ;
WO 2010/094242 A1
反应条件
1: 98 percent / CuI; Pd(PPh3) / various solvent(s) / 0.5 h / 20 °C
2: 99.8 percent / 1,4-cyclohexadiene / 10 percent Pd/C / ethanol / 1 h / 0 - 20 °C
3: 97 percent / 4-methylmorpholine-N-oxide; 4 Angstroem m. s.; TPAP / CH2Cl2 / 0.17 h
4: 85 percent / potassium t-butoxide / dioxane / 1 h / 20 °C
5: 99.8 percent / 2M HCl / propan-2-ol; tetrahydrofuran / 1 h / 20 °C
6: 87 percent / potassium nitrosodisulfonate (Fremy's salt); NaH2PO4*H2O; Aliquat 336 / H2O; CH2Cl2
View Scheme
参考文献
Hadfield, John A.; McGown, Alan T.; Butler, John
Molecules, 2000 , vol. 5, # 1 p. 82 - 88
反应条件
1: 94 percent / triphenylphosphine; triethylamine; copper(I) iodide / bis(triphenylphosphine)palladium(II) chloride / 80 °C
2: 78 percent / sodium hydroxide / toluene / 3.5 h / Heating
View Scheme
参考文献
Tsang, Kit Y.; Brimble, Margaret A.; Bremner, John B.
Organic Letters, 2003 , vol. 5, # 23 p. 4425 - 4427
