CaH2 in toluene byproducts: H2; react. under N2, slow addn. of the alcohol via syringe to B(OH)3 and CaH2, cooling in a water bath, slow heating to 80-90°C for 24 h after abating the H2 gas evolution; distn. of the volatile products under reduced pressure (distn. pot temp. <= 120°C), extn. with hot toluene or cyclohexane under N2;
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
phenol in toluene byproducts: H2O; azeotropic removal of H2O in refluxing toluene;
参考文献
Perchenko, V. N.; Abubakirov, R. Sh.; Kurashev, M. V.; Semenov, O. B.; Khrapova, I. M.; Plate, N. A.
Doklady Chemistry, 1992 , vol. 326, # 1.3 p. 191 - 193
Dokl. Akad. Nauk SSSR Ser. Khim., 1992 , vol. 326, # 2 p. 276 - 278
ethanol in benzene a mixt. of ethanol, benzene, orthoboric acid, and anhydrous CuSO4 is boiled on a Dean-Stark apparatus with driving off water (40-50 h);; repeated fractional distn.;;
参考文献
Gertsev, V. V.; Romanov, Yu. A.
Journal of Applied Chemistry USSR (English Translation), 1992 , vol. 65, p. 314 - 318
Zhurnal Prikladnoi Khimii (Sankt-Peterburg, Russian Federation), 1992 , vol. 65, p. 375 - 380
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
