Technology Process of [(Me3SiN=PPh2)2C=Ge→Ge=C(PPh2=NSiMe3)2]
There total 4 articles about [(Me3SiN=PPh2)2C=Ge→Ge=C(PPh2=NSiMe3)2] which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
toluene;
under N2 atm. soln. (HC(PPh2=NSiMe3)2GeCl) in toluene was added to stirred soln. (Ge(N(SiMe3)2)2) in toluene at room temp. and stirred for 2 days; volatiles were removed under reduced pressure, residue was extd. with hexane/Et2O (1:1), soln. was filtered and concd.;
DOI:10.1021/om034071t
- Guidance literature:
-
With
[CH((C6H5)2PNSi(CH3)3)2Li(thf)];
In
diethyl ether;
byproducts: CH2((C6H5)2PNSi(CH3)3)2; soln. of lithium salt (with two equivs.) added to cooled (-90°C) suspn. of GeCl2*dioxane with stirring; mixt. stirred at room temp. for 18 h, then filtered; then 20 mL hexane added to filtrate, soln. concd. toabout 5 mL; mixt. stood for 5 d; elem.anal.; detd. by NMR spectroscopy, X-ray crystallography;
DOI:10.1002/1521-3773(20010702)40:13<2501::AID-ANIE2501>3.0.CO;2-Q
- Guidance literature:
-
In
diethyl ether;
under N2 atm. soln. (HC(PPh2=NSiMe3)2Li*THF) in Et2O was added slowly at-90°C to stirred soln. GeCl2*dioxane in Et2O, temp. was raised t o room temp. and stirred for 2 days; ppt. was filtered, hexane was added to filtrate and concd. under reducedpressure;
DOI:10.1021/om034071t