2,4-二氯-3-甲基苯甲酸合成路线 （共 8 条）
反应条件
1: 2,4-dichloro-6-methylbenzoic acid; 2,4-Dichloro-3-methyl-benzoic acid With oxalyl dichloride; N,N-dimethyl-formamide in dichloromethane T=0°C; 1 - 2 h; 2: methanol 16 h; 3: With N-bromosuccinmide; dibenzoyl peroxide in tetrachloromethane 5 h; Heating / reflux;
参考文献
GLAXO GROUP LIMITED
Patent: WO2004/89897 A1, 2004 ;
Location in patent: Page 19; 20; 26 ;
WO 2004/089897 A1
反应条件
1: With potassium hydroxide; water in tetrahydrofuran; methanol
T=45°C; 1 h;
2: With hydrogenchloride in tetrahydrofuran; methanol; water
参考文献
GLAXO GROUP LIMITED
Patent: WO2004/89897 A1, 2004 ;
Location in patent: Page 20 ;
WO 2004/089897 A1
反应条件
sodium hydroxide; bromine in 1,4-dioxane; water
参考文献
BASF Aktiengesellschaft
Patent: US6576596 B1, 2003 ;
反应条件
1: 2,6-dichlorotoluene With 2,2,6,6-tetramethyl-piperidine; n-butyllithium in tetrahydrofuran
T=-78°C; Inert atmosphere;
2: carbon dioxide in tetrahydrofuran
T=20°C; 4 h;
参考文献
GLAXO GROUP LIMITED; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; SIME, Mairi; STEADMAN, Jon Graham Anthony; THEWLIS, Rachel Elizabeth Anne; TRANI, Giancarlo; WALTER, Daryl Simon
Patent: WO2010/125102 A1, 2010 ;
Location in patent: Page/Page column 100 ;
WO 2010/125102 A1
反应条件
1: 2,4-dichloro benzoic acid With sec.-butyllithium in tetrahydrofuran; cyclohexane
T=-78°C; 1 h;
2: methyl iodide in tetrahydrofuran; cyclohexane
T=-78 - 25°C; 4 h;
3: With hydrogenchloride; water
more than 3 stages;
参考文献
GLAXO GROUP LIMITED
Patent: WO2004/89897 A1, 2004 ;
Location in patent: Page 19; 20; 26 ;
WO 2004/089897 A1
反应条件
sodium hydroxide; bromine in 1,4-dioxane; water
参考文献
BASF Aktiengesellschaft
Patent: US6372693 B1, 2002 ;
反应条件
1: 2,6-dichlorotoluene With sec.-butyllithium in tetrahydrofuran; cyclohexane
T=-75°C; 0.75 h;
2: carbon dioxide in tetrahydrofuran; cyclohexane
Title compound not separated from byproducts;
参考文献
Schlosser, Manfred; Heiss, Christophe; Marzi, Elena; Scopelliti, Rosario
European Journal of Organic Chemistry, 2006 , # 19 p. 4398 - 4404
反应条件
oxygen; antimony trichloride; chlorine
T=95°C; 3 h; multistep reaction; other temp., time; Product distribution;
参考文献
Uvarova, I. P.; Golod, L. P.; Yazlovitskii, A. V.; Rudenko, S. D.; Shcherbina, F. F.; Girgor'ev, A. A.
J. Appl. Chem. USSR (Engl. Transl.), 1990 , vol. 63, # 2.2 p. 483 - 486,463 - 465
