Technology Process of 12-bromo-N-phenyl-5,6,7,12-tetrahydrodibenz[c,f][1,5]azastibocine
There total 1 articles about 12-bromo-N-phenyl-5,6,7,12-tetrahydrodibenz[c,f][1,5]azastibocine which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
n-BuLi;
In
diethyl ether; hexane;
under Ar; ligand disolved in Et2O; cooled in methanol-ice bath (-15 to -20 degree.C); n-BuLi in hexane added; stirred for 1 h; etherial soln. ofSbBr3 added; stirred at room temp. for 12 h; quenched with H2O; diluted with CHCl3; org. layer sepd.; washed with satd. aq. NaHCO3 and brine; dried (anhyd. MgSO4); removed in vac.; purifiedby column chromy. (silica gel, CH2Cl2-ethyl acetate 4:1); recrystd. fro m CHCl3-EtOH; elem. anal.;
DOI:10.1016/j.jorganchem.2006.02.041
- Guidance literature:
-
With
n-BuLi;
In
tetrahydrofuran; diethyl ether; hexane;
under Ar; n-BuLi in hexane added at 0°C to stirred soln. of PhCCHin Et2O; stirred for 1 h; THF soln. of Sb compd. added dropwise at 0.de gree.C; stirred for 4 h; diluted with ether; quenched with H2O; ether layer sepd.; washed with brine; dried (anhyd. MgSO4); concd. in vac.; purified by column chromy. (silica gel, hexane-ethyl acetate 1:1); recrystd. from benzene-hexane; elem. anal.;
DOI:10.1016/j.jorganchem.2006.02.041
