2,6-二氯-4-羟基苯甲醛合成路线 (共 11 条)
反应条件
1: 3-chloro-5-[(triisopropylsilyl)oxy]phenyl chloride With n-butyllithium in tetrahydrofuran; hexane T=-78°C; 0.75 h; 2: N,N-dimethyl-formamide in tetrahydrofuran; hexane T=-78 - -10°C; 3: With hydrogenchloride in tetrahydrofuran; hexane; water
参考文献
INCYTE CORPORATION
Patent: WO2007/38215 A1, 2007 ;
Location in patent: Page/Page column 106-107 ;
WO 2007/038215 A1
反应条件
1: 1-lt;(tert-butyldimethylsilyl)oxygt;-3,5-dichlorobenzene With sec.-butyllithium in tetrahydrofuran T=-70 - -68°C; 2.25 h; 2: N,N-dimethyl-formamide in tetrahydrofuran T=-70°C; 1 h; 3: With hydrogenchloride; water in tetrahydrofuran T=20°C;
参考文献
Aicher, Thomas Daniel; Anzeveno, Peter Biagio; Li, Renhua; Krasutsky, Alexei Pavlovych; Mabry, Thomas Edward; Saeed, Ashraf; Snyder, Nancy June; Stephenson, Gregory Alan; Tian, Hongqi; Wallace, Owen Brendan; Winneroski, JR., Leonard Larry; Xu, Yanping
Patent: US2009/111800 A1, 2009 ;
Location in patent: Page/Page column 26 ;
US 20090111800 A1
反应条件
1: 3-chloro-5-[(triisopropylsilyl)oxy]phenyl chloride With n-butyllithium in tetrahydrofuran; hexane T=-70 - -65°C; 2 h; 2: N,N-dimethyl-formamide in tetrahydrofuran; hexane T=-65 - 20°C;
参考文献
WO2005/40154 A1, ;
Page/Page column 24 ;
WO 2005/040154 A1
反应条件
1.1: 100 percent / 2,6-lutidine / CH2Cl2 / 2 h / 0 °C 2.1: n-BuLi / hexane; tetrahydrofuran / 0.75 h / -78 °C 2.2: hexane; tetrahydrofuran / -65 - -10 °C 3.1: 4.37 g / aq. HCl; NaCl View Scheme
参考文献
Synthesis, , # 12 p. 2062 - 2065
反应条件
1: 3-chloro-5-[(triisopropylsilyl)oxy]phenyl chloride With n-butyllithium in tetrahydrofuran; hexane T=-70 - -65°C; 2 h; 2: N,N-dimethyl-formamide in tetrahydrofuran; hexane T=-65 - 20°C; 3: With hydrogenchloride in tetrahydrofuran; hexane; water T=20°C; 1 h; Product distribution / selectivity;
参考文献
US2003/199691 A1, ;
Page/Page column 6 ;
反应条件
1: 3-chloro-5-[(triisopropylsilyl)oxy]phenyl chloride With n-butyllithium in tetrahydrofuran; hexane T=-78 - -67°C; 0.75 h; 2: N,N-dimethyl-formamide in tetrahydrofuran; hexane T=-65 - -10°C; 3: With hydrogenchloride in tetrahydrofuran; hexane; water Product distribution / selectivity;
参考文献
US2003/199691 A1, ;
Page/Page column 6 ;
反应条件
calcium hydroxide powder; sodium carbonate in water 2 h; Heating;
参考文献
Knuutinen, Juha S.; Kolehmainen, Erkki T.
Journal of Chemical & Engineering Data, 1983 , vol. 28, # 1 p. 139 - 141
反应条件
1.1: HCl; H2SO4 / H2O / 60 °C 1.2: 30 percent / NaOH / dioxane; H2O / 3 h / Heating 2.1: MnO2 / benzene / Heating 3.1: BBr3 / CH2Cl2 / 0 - 20 °C View Scheme
参考文献
Bioorganic and medicinal chemistry, , vol. 11, # 16 p. 3457 - 3474
反应条件
1: MnO2 / benzene / Heating 2: BBr3 / CH2Cl2 / 0 - 20 °C View Scheme
参考文献
Bioorganic and medicinal chemistry, , vol. 11, # 16 p. 3457 - 3474
反应条件
sodium tetrahydroborate; water in ethanol
1 h;
参考文献
Woo, L. W. Lawrence; Wood, Paul M.; Bubert, Christian; Thomas, Mark P.; Purohit, Atul; Potter, Barry V. L.
ChemMedChem, 2013 , vol. 8, # 5 p. 779 - 799