Technology Process of (HCCCHO)Co2(CO)5(PPh3)
There total 2 articles about (HCCCHO)Co2(CO)5(PPh3) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
tetrahydrofuran;
under N2; Co-contg. compd. (0.59 mmol), PPh3 (0.59 mmol), and THF were added to a Schlenk flask; the mixt. was heated at reflux for 3 h; coolingto room temp.; solids were filtered off and the filtrate was evapd. to dryness; column chromy. (silica gel, C6H14 and Et2O (v/v, 3:1)); the solvent was removedby a rotary evaporator; keeping in vac. for a day; elem. anal.;
DOI:10.1016/S0020-1693(02)01185-4
- Guidance literature:
-
With
oxalyl chloride; Et3N;
In
dichloromethane; dimethyl sulfoxide;
under N2; to the DMSO (activated with oxalyl chloride) in CH2Cl2 was added Co-contg. compd. at -78°C; stirring for 15 min at -78°C; then Et3N was added; the soln. was allowed to warm to room temp. for 40 min; CH2Cl2 and NH4Cl soln. were added; the CH2Cl2 layer was chromd. on a silica gel column eluting with C6H14 and Et2O (5:1); removal of the solvent; optically pure compd. was prepd.;
DOI:10.1016/S0020-1693(02)01185-4
- Guidance literature:
-
With
catalyst: 18-crown-6; (t)BuOK;
In
tetrahydrofuran;
under N2; (4-nitrobenzyl)triphenylphosphonium bromide (1.0 mmol) and (t)BuOK (1.4 mmol) in THF were stirred with catalytic amt. of 18-crown-6 for 1 h; then optically pure Co-contg. compd. (0.70 mmol) was added; stirring for 5 h; excess CH2Cl2 and satd. aq. NaCl soln. were added; the CH2Cl2 layer was chromd. on a silica gel column with C6H14 and Et2O (5:1); then the solvent was removed; optically pure compd. was prepd.;
DOI:10.1016/S0020-1693(02)01185-4
