2-甲基-1,3,2-二氧硼杂环己烷合成路线 (共 5 条)
反应条件
hydrogenchloride in diethyl ether byproducts: LiCl; 2 equiv of MeLi slowly adding to a soln. of the boronic ester at -78°C, stirring for 3 h at the same temp., 1 equiv of anhydrous HCl in Et2O adding, warming to room temp., stirring for 15 min; the content was detd. by (11)B NMR spectrum;
参考文献
Organometallics, , vol. 4, p. 1788 - 1792
反应条件
hydrogenchloride; methylmagnesium bromide in diethyl ether
(N2); a soln. of B-compound cooled with a dry ice-acetone bath; a soln.of CH3MgBr added dropwise via syringe; stirred for 0.5 h; allowed to warm to room temp. with stirring for 0.5 h; cooled to 0°C; a soln. of HCl in ether added; warmed to room temp.; detected by (11)B NMR;
参考文献
Brown, Herbert C.; Cole, Thomas E.
Organometallics, 1985 , vol. 4, p. 816 - 821
反应条件
hydrogenchloride; methylmagnesium bromide in diethyl ether
byproducts: (CH3)3B, Li(CH3)4B; (N2); a soln. of B-compound cooled with a dry ice-acetone bath; a soln.of CH3MgBr added dropwise via syringe; stirred for 0.5 h; allowed to warm to room temp. with stirring for 0.5 h; cooled to 0°C; a soln. of HCl in ether added; warmed to room temp.; detected by (11)B NMR;
参考文献
Brown, Herbert C.; Cole, Thomas E.
Organometallics, 1985 , vol. 4, p. 816 - 821
反应条件
hydrogenchloride; methylmagnesium bromide in diethyl ether
(N2); a soln. of B-compound cooled with a dry ice-acetone bath; a soln.of CH3MgBr added dropwise via syringe; stirred for 0.5 h; allowed to warm to room temp. with stirring for 0.5 h; cooled to 0°C; a soln. of HCl in ether added; warmed to room temp.; detected by (11)B NMR;
参考文献
Brown, Herbert C.; Cole, Thomas E.
Organometallics, 1985 , vol. 4, p. 816 - 821
反应条件
methanesulfonic acid in tetrahydrofuran
dropwise addn. of CH3Li (1 equiv.) to soln. of C6H11B(OC3H6O) (2.5 mmol) in THF at -78°C via syringe; stirring at -78°C for 3 h; addn. of CH3SO3H at -78/25°C; warming slowly to room temp.; stirring at room temp.;; not isolated; product distribution (depending on temp. at which acid is added) is determined by 11B-NMR;;
参考文献
Brown, Herbert C.; Vasumathi, Nagarajan; Joshi, Navalkishore N.
Organometallics, 1993 , vol. 12, p. 1058 - 1067