Technology Process of 3-phenyl-4-(tri-n-butylstannyl)-3-cyclobutene-1,2-dione-1-ethylene acetal
There total 1 articles about 3-phenyl-4-(tri-n-butylstannyl)-3-cyclobutene-1,2-dione-1-ethylene acetal which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
n-butyllithium;
In
tetrahydrofuran; hexane;
reaction of CuCN in THF with n-C4H9Li in hexane at -78°C, stannane added, stirred at -78°C for 20 min, warmed to room temp., stirred for 90 min, cooled to -78°C, THF-soln. of acetal added dropwise, stirred for 1 h at -78°C; quenched at -78°C (satd. NH4Cl-soln.), warmed to room temp., added to H2O, extd. (ether), organic layers washed (water, brine), dried (Na2SO4), filtered, solvent removed, chromd. (SiO2, 1:32 EtOAc/hexanes);
DOI:10.1021/ja00073a021
- Guidance literature:
-
With
sulfuric acid;
In
tetrahydrofuran; water;
acetal was dissolved in THF, cooled to 0°C, 50% aq. H2SO4 was added, stirred at 0°C. for 2.5 h; diluted (ether), water added, water layer separated and extd. (ether), organic layers washed (satd. NaHCO3-soln.), aq. layer extd. (ether), organic layers dried (Na2SO4), filtered, solvent removed, chromd. (SiO2, EtOAc/hexanes 1:10);
DOI:10.1021/ja00073a021
