Technology Process of 1-(phenylethynyl)germatrane
There total 2 articles about 1-(phenylethynyl)germatrane which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
Et3N; EtOH;
In
ethanol; toluene;
(N2); standard Schlenk technique; flask with mixt. of C6H5CCH, GeCl4, Et3N in toluene was sealed, cooled, evacuated; heated at 110°C for 21 h; filtered; residue washed (toluene); EtOH and Et3N were added to filtrate and washings; mixt. stirred at; room temp. for 50 min; filtered; residue washed (toluene); filtrate and washings were added to (HOCH2CH2)3N; mixt. was stirred at 110°C for 6 h; cooled to room temp.; filtered; washed (pentane; CH2Cl2); solvent removed (vac.);
DOI:10.1021/om020578c
- Guidance literature:
-
In
tetrahydrofuran; toluene;
byproducts: LiBr; (Ar); addn. of a soln. of lithium compd. in THF to a suspn. of germatrane in toluene at room temp., stirring for 24 h at room temp.; concmn., filtration, evapn., addn. of pentane, keeping at -30°C for 20 h, filtration, drying in vac., sublimation (100°C/0.05 Torr); elem. anal.;
DOI:10.1016/S0022-328X(01)00708-2
- Guidance literature:
-
In
dimethyl sulfoxide;
addn. of NBS to a soln. of germatrane in DMSO, stirring at room temp. for 24 h; addn. of water, extn. with CHCl3, washing with water, drying with MgSO4,evapn., recrystn. (CHCl3/hexane), drying in vac.; elem. anal.;
DOI:10.1016/S0022-328X(01)00708-2
