in diethylene glycol dimethyl ether
addn. of BF3*OEt2 to NaBH4 in diglyme over 2 h, sweeping the B2H6 formedwith an N2 stream into the nitrile at 60°C; sepn. by distn.; elem. anal.;
参考文献
Coult, Robert; Fox, Mark A.; Rand, Brian; Wade, Kenneth; Westwood, Aidan V. K.
Journal of the Chemical Society - Dalton Transactions, 1997 , # 19 p. 3411 - 3413
in neat (no solvent)
byproducts: (C2H5)2O; heating equimolar mixt. of BF3*(C2H5)2O and As2O3;;
参考文献
Fofanova, E. L.; Gavrilov, V. I.; Garieva, F. R.; Musin, R. Z.
Journal of General Chemistry USSR (English Translation), 1992 , vol. 62, p. 922 - 924
Zhurnal Obshchei Khimii, 1992 , vol. 62, p. 1127 - 1129
in neat (no solvent)
byproducts: (C2H5)2O; heating equimolar mixt. of BF3*(C2H5)2O and (C5H11O)3As;;
参考文献
Fofanova, E. L.; Gavrilov, V. I.; Garieva, F. R.; Musin, R. Z.
Journal of General Chemistry USSR (English Translation), 1992 , vol. 62, p. 922 - 924
Zhurnal Obshchei Khimii, 1992 , vol. 62, p. 1127 - 1129
in diethyl ether
dropwise addn. of 4-picoline soln. to BF3 ether complex with stirring; filtration; washing with dry ether; elem. anal.;
参考文献
Vasil'ev, A. N.; Mushkalo, L. K.
Journal of General Chemistry USSR (English Translation), 1992 , vol. 62, p. 1718 - 1720
Zhurnal Obshchei Khimii, 1992 , vol. 62, p. 2087 - 2090
Al; HgCl2 in diethyl ether
under N2 atm.; to Al, HgCl2 dry N2 purged Et2O added; soln. stirred, heated to 35°C; CH2CHCH2Br added slowly dropwise; mixt. stirred at reflux at 67°C for 3 h; transferred in the flask contg. BF3*Et2O; soln. refluxed at 70°C for 3 h; Et2O removed by short-path distn. under N2; residue distd. (vac. 20 mmHg) with a short-path distn. head at a head temp. of 65°C; monitored by NMR; second vac. distn.;
参考文献
Wagner, Carl E.; Kim, Jang-Seob; Shea, Kenneth J.
Journal of the American Chemical Society, 2003 , vol. 125, # 40 p. 12179 - 12195
