in tetrahydrofuran; diethyl ether; benzene
N2; MeLi in ether added to diene in THF at -78°C, after 2 min MgBr2*OEt2 in ether/benzene; poured into Ph2S2 in THF at -78°C; bath removed; stirred for 2.25 h;; poured into NaOH and ether/pentane; organic layer washed with water and brine; filtered through Na2SO4; radical inhibitor added; solvent removed; preparative TLC (50/1 pentane/ether);;
参考文献
Reich, Hans J.; Reich, Ieva L.; Yelm, Kenneth E.; Holladay, Johnathan E.; Gschneidner, David
Journal of the American Chemical Society, 1993 , vol. 115, # 15 p. 6625 - 6635
in diethyl ether
(Ar); to a soln. of 3,4,8-trimethyl-3-borabicyclo(4.3.1)decane was added at -60°C MeLi in ether; heating to 20°C, then cooled to -10 to 0°C; AcCl was added to the mixt.; stirred for 1 h at 20°C; ether was distd. off, and pentane was added to the residue; the ppt. was filtered off, and the solvent was removed from the filtrate; distn. of the residue gave 2-(3-methylene-5-methylcyclohex-1-yl)propyl(dimethyl)borane; elem. anal.;
参考文献
Gurskii, M. E.; Baranin, S. V.; Lutsenko, A. I.; Mikhailov, B. M.
Journal of Organometallic Chemistry, 1984 , vol. 270, # 1 p. 17 - 24
in tetrahydrofuran; N,N,N',N',N'',N''-hexamethylphosphoric triamide
treatment of the corresponding (Z)-2,3-bis(trimethylstannyl)-2-alkenoate with MeLi in THF-HMPA (-98°C, 20 min);
参考文献
Piers, Edward
Pure and Applied Chemistry, 1988 , vol. 60, p. 107 - 114
