in dichloromethane
addn. of BF3*OEt2 to soln. of 1,3-diketone in dichloromethane at room temp., reaction mixture remained for 72 h at room temp.; evapn. in vac., residue suspended in water, solid material filtered off and recryst. from toluene; elem. anal.;
参考文献
Stefane, Bogdan; Polanc, Slovenko
New Journal of Chemistry, 2002 , vol. 26, # 1 p. 28 - 32
potassium permanganate; sulfuric acid in water; diethylene glycol; benzene
byproducts: H2; NaBH4 in diglyme heated to 105°C and BF3*OEt2 added for 6 h and stirred for 1 h, mixt. cooled under N2 atm., water added, diglyme removed, H2SO4, benzene and KMnO4 added and react. mixt. stirred at 10°C; mixt. filtered, layers separated, benzene layer washed with water and dried over anhyd. MgSO4, evapd. and sublimed;
参考文献
Dunks, Gary B.; Barker, Kathryn; Hedaya, Eddie; Hefner, Catherine; Palmer-Ordonez, Kathy; Remec, Peter
Inorganic Chemistry, 1981 , vol. 20, p. 1692 - 1697
in diethyl ether
byproducts: LiF; heating at 120-130°C several h, cooling, dissolving in ether, decanting, solvent evapn.; recrystn. from anhydrous ether;
参考文献
Gmelin Handbook: B: B-Verb.8, 1.2, page 2 - 5
Full Text Show Details
Becher, H. J.
in: G. Brauer, Handbuch der Praeparativen Anorganischen Chemie, 2. Edn., Vol. 1, Ferdinand Enke, Stuttgart 1960, pp.689/91
