CaH2 in neat (no solvent) byproducts: H2; react. under N2, slow addn. of the alcohol via syringe to B(OH)3 (ratio 3:1) and CaH2, cooling in a water bath, slow heating to 80 - 90°C for 12 h after abating the H2 gas evolution; distn. of the volatile products under reduced pressure (distn. pot temp. <= 120°C);
参考文献
Cole, T. E.; Quintanilla, R.; Rodewald, S.
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 1990 , vol. 20, p. 55 - 64
CaH2 in cyclohexane byproducts: H2; react. under N2, slow addn. of the alcohol to the trialkoxyboroxine and CaH2 in cyclohexane, cooling in a water bath, rapid gas evolution, stirring for 1 h at room temp., heating to 80-90°C overnight; distn. of the product under reduced pressure;
参考文献
Cole, T. E.; Quintanilla, R.; Rodewald, S.
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 1990 , vol. 20, p. 55 - 64
in pentane byproducts: H2; (Ar (N2) or vac.); dropwise addn. of excess of i-PrOH to Hf-complex in pentane with stirring (60 min, room temp.); concn., filtration, drying (vac.); elem. anal.;
参考文献
Petrova, L. A.; Borisov, A. P.; Makhaev, V. D.
Sov. J. Coord. Chem. (Engl. Transl.), 1992 , vol. 18, p. 425 - 428
Koordinatsionnaya Khimiya, 1992 , vol. 18, p. 492 - 496
in benzene byproducts: H2O; under Ar, soln. of allylboronic acid in C6H6 treated with 2-propanol (2 equiv), heated to reflux until evolution of H2O completed (Dean-Stark trap); fractionally distd. (bp 62-64°C, 40 mmHg);
参考文献
Journal of the American Chemical Society, , vol. 107, # 26 p. 8186 - 8190
acetyl chloride in diethyl ether dropwise addn. of EtMgBr (1-2.5 equiv.) to soln. of C6H11B(OCH(CH3)2)2 (2.5 mmol) in ether at -78°C via syringe; stirring at -78°C for 3 h; addn. of CH3COCl at -78°C; warming slowly to room temp.; stirring (room temp.);; not isolated; product distribution is determined by 11B-NMR;;
methanesulfonic acid in tetrahydrofuran dropwise addn. of i-BuMgBr (2 equiv.) to soln. of C6H11B(OCH(CH3)2)2 (2.5 mmol) in THF at -78°C via syringe; stirring at -78°C for 3 h; addn. of CH3SO3H at -78°C; warming slowly to room temp.; stirring at room temp.;; not isolated; product distribution is determined by 11B-NMR;;
CH3SO3H or HCl or CH3COCl or ClCH2COCl or Cl3CCOCl in diethyl ether addn. of CH3Li to soln. of C6H11B(OCH(CH3)2)2 (2.5 mmol) in ether at -78°C via syringe; stirring at -78°C for 3 h; addn. of acid (further acids investigated: ClCH2COCl, (CH3)3SiCl); warming slowly to room temp.; stirring at room temp.;; not isolated; product distribution is determined by 11B-NMR for various conditions (temp. at which acid is added, amt. of CH3Li, amt. of acid);;
methanesulfonic acid in tetrahydrofuran dropwise addn. of EtMgBr (1-3 equiv.) to soln. of C6H11B(OCH(CH3)2)2 (2.5 mmol) in THF at -78°C via syringe; stirring at -78°C for 3 h; addn. of CH3SO3H at -78°C; warming slowly to room temp.; stirring (room temp.);; not isolated; product distribution is determined by 11B-NMR;;
