Technology Process of Zr(PhN(CH2)3NPh)Cl2(THF)2
There total 1 articles about Zr(PhN(CH2)3NPh)Cl2(THF)2 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
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In
diethyl ether;
byproducts: LiCl; N2 atm.; THF and diethyl ether were vac.-transfered at -196°C to the mixt. of Li-compound and ZrCl4, stirred for 27 h in an ice bath at 0°C, volatiles removed, C6H6 was added, stirred for 2 h at room temp.; filtered, vac.-evapd., toluene-soln. was stirred overnight, filtered, passed through Celite column, concd. at 35°C under vac., THF-soln. was stirred for 1 h, hexane was added, stirred, cooled to -35°C for 24 h, filtered, dried under vac.;
DOI:10.1021/ja046629+
- Guidance literature:
-
In
diethyl ether;
N2 atm.; diethyl ether was vac.-transfered into the flask with complex and Li-compound at -196°C, allowed to warm to room temp., stirred for 19 h; volatiles were removed under vac., taken up in benzene, stirred for 15 min at room temp., filtered, volatiles were removed under vac. at 30°C for 2 h, recrystd. from benzene-hexane; elem. anal.;
DOI:10.1021/ja046629+
- Guidance literature:
-
In
diethyl ether;
under N2 atm. to Li2(Me2Si(3-(t)Bu-C5H3)2) and Zr(PhN(CH2)3NPh)Cl2(THF)2at -196°C Et2O was added, react. mixt. was warmed to 0°C, stirred for 6 h, warmed to room temp. and stirred overnight; volatiles were removed in vacuo at 25°C, toluene was added at -196°C, warmed to room temp. and stirred for 30 min, soln. was filtered, volatiles were removed in vacuo at 25°C, residue was dried in vacuo; elem. anal.;
DOI:10.1021/om034184c
