Technology Process of (Re(CO)4(CON(Ph)C(Me)NPh))
There total 2 articles about (Re(CO)4(CON(Ph)C(Me)NPh)) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
n-butyllithium;
In
1,2-dimethoxyethane; hexane;
byproducts: lithium bromide, Re(CO)3(PhNCMeNPh)(PhNHCMeNPh); under N2 atm. to soln. PhNHC(Me)NPh in monoglyme (-196°C) added soln. n-butyl-lithium in hexane, mixt. allowed to room temp. and stirredfor 15 min, soln. refrozen, (Re(CO)5Br) added, warmed to room temp. andstirred for 2.5 h; soln. reduced, hexane added, mixt. cooled to -10°C, filtered, evapd. to dryness, residue extd. with CH2Cl2, filtered through alumina, reduced in volume, ether added, soln. cooled - (Re(CO)4(COL)), hexane added - (Re(CO)3L(HL)); elem. anal.;
- Guidance literature:
-
With
n-butyllithium;
In
1,2-dimethoxyethane; hexane;
byproducts: lithium bromide; under N2 atm. to soln. PhNHC(Me)NPh in monoglyme (-196°C) added soln. n-butyl-lithium in hexane, mixt. allowed to room temp. and stirredfor 15 min, soln. refrozen, (Re(CO)5Cl) added, warmed to room temp. andstirred for 2.5 h; soln. reduced, hexane added, mixt. cooled to -10°C, filtered, evapd. to dryness, residue extd. with CH2Cl2, filtered through alumina, reduced in volume, ether added, soln. cooled - (Re(CO)4(COL)), hexane added - (Re(CO)3L(HL)); elem. anal.;
- Guidance literature:
-
With
triphenylphosphine;
In
1,2-dimethoxyethane;
mixt. complex and triphenylphosphine dissolved in monoglyme and soln. refluxed for 27 h; soln. evapd.;