2,2-二甲基-1,3-丙二醇合成路线 （共 467 条）
反应条件
in dichloromethane
all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
参考文献
Yasuike, Shuji; Nakata, Kazuhide; Qin, Weiwei; Kaji, Toshiyuki; Kurita, Jyoji
Chemistry Letters, 2006 , vol. 35, # 12 p. 1402 - 1403
反应条件
1.1: NaH / tetrahydrofuran / 14 h / 20 °C
2.1: 39.8 g / SO3*py; NEt3; DMSO / CH2Cl2; dimethylsulfoxide / 9 h / 20 °C
3.1: MeMgCl / tetrahydrofuran / -78 - 10 °C
3.2: Mg; 1,2-dibromo-ethane / tetrahydrofuran / 14.5 h / Heating
3.3: tetrahydrofuran / 0.5 h / -78 °C
4.1: (COCl)2; DMSO; Et3N / CH2Cl2 / -78 °C
View Scheme
参考文献
Wender, Paul A.; Baryza, Jeremy L.; Bennett, Chad E.; Bi, F. Christopher; Brenner, Stacey E.; Clarke, Michael O.; Horan, Joshua C.; Kan, Cindy; Lacote, Emmanuel; Lippa, Blaise; Nell, Peter G.; Turner, Tim M.
Journal of the American Chemical Society, 2002 , vol. 124, # 46 p. 13648 - 13649
反应条件
1: 3-hydroxy-2,2-dimethylpropanol With tetrakis(dimethylamino)diboron; potassium acetate in toluene
T=80°C; 0.5 h;
2: 1-trifluoromethyl-4-bromobenzene With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride in toluene
T=80°C; 22 h; Reagent/catalystTime;
参考文献
BASF SE; SCHMIDT-LEITHOFF, Joachim; PICHLMAIR, Stefan; BELLO, Charles; BASF (CHINA) COMPANY LIMITED
Patent: WO2013/14579 A1, 2013 ;
Location in patent: Page/Page column 11; 12; 13 ;
反应条件
in toluene
RefluxInert atmosphere;
参考文献
Berini, Christophe; Navarro, Oscar
Chemical Communications, 2012 , vol. 48, # 10 p. 1538 - 1540
反应条件
1: potassium acetate / 80 °C
2: (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / toluene / 22 h / 80 °C
View Scheme
参考文献
Bello, Charles S.; Schmidt-Leithoff, Joachim
Tetrahedron Letters, 2012 , vol. 53, # 46 p. 6230 - 6235,6
反应条件
1: tetrakis(dimethylamino)diboron; 3-hydroxy-2,2-dimethylpropanol With potassium acetate in toluene
T=80°C;
2: 4-nitrophenyl trifluoromethanesulphonate With tetrakis(triphenylphosphine) palladium(0) in toluene
T=80°C; 22 h;
参考文献
Bello, Charles S.; Schmidt-Leithoff, Joachim
Tetrahedron Letters, 2012 , vol. 53, # 46 p. 6230 - 6235,6
反应条件
1: potassium acetate / 80 °C
2: tetrakis(triphenylphosphine) palladium(0) / toluene / 3 h / 80 °C / |Inert atmosphere
View Scheme
参考文献
Bello, Charles S.; Schmidt-Leithoff, Joachim
Tetrahedron Letters, 2012 , vol. 53, # 46 p. 6230 - 6235,6
反应条件
in diethyl ether
T=20°C; 6 h; Inert atmosphereSchlenk techniqueGreen chemistry;
参考文献
Wang, Wenlong; Zhang, Guodong; Lang, Rui; Xia, Chungu; Li, Fuwei
Green Chemistry, 2013 , vol. 15, # 3 p. 635 - 640
反应条件
1: 96 percent / pyridine
2: 71 percent / ethane-1,2-diol / 2 h / Heating
3: 85 percent / NaOH / H2O / 48 h / Heating
4: 89 percent / Thionyl chloride
View Scheme
参考文献
Wills, Max T.; Wills, Irene E.; Dollen, Lawrence Von; Butler, Barry L.; Porter, John; Anderson, Arthur G.
Journal of Organic Chemistry, 1980 , vol. 45, # 12 p. 2489 - 2498
反应条件
diboron trioxide in benzene
参考文献
Wolf,P.F. et al.
Journal of Organic Chemistry, 1975 , vol. 40, p. 1875 - 1882
