Technology Process of cyclohexylcarbonyltriethylgermane
There total 1 articles about cyclohexylcarbonyltriethylgermane which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
oxalyl dichloride; dimethyl sulfoxide; triethylamine;
In
dichloromethane;
under Ar, addn. of DMSO in CH2Cl2 to oxalyl chloride in CH2Cl2 at -50 - -60°C, stirring for 2 min, addn. of the germane in CH2Cl2 during 5 min, stirring for 15 min, addn. of NEt3, allowed to warm to room temp. after 5 min, stirring for 3 h; quenching the react. with H2O, sepn. of the org. layer, extn. the aq. layer (CH2Cl2), combined extracts washed (H2O and satd. aq. NaCl), dried (MgSO4), concg., column. chromy (silica gel, hexane-ethyl acetate 50:1), elem. anal.;
- Guidance literature:
-
In
tetrahydrofuran;
under Ar, addn. of a soln. of the germane in THF to a soln. of the Li phenyl sulfone (prepd. from the sulfone and lithium diisopropylamide) in THF, stirring at -78°C for 10 min, then at 0°C for 0.5 h, quenching the react. with aq. NH4Cl; sepn. of the org. layer, extn. of the aq. layer (ether), washing the combined extracts (H2O and satd. aq. NaCl), drying (MgSO4), concg., column chromy. (silica gel, hexane-ethyl acetate 20:1), elem. anal.;
- Guidance literature:
-
In
tetrahydrofuran;
under Ar, addn. of a soln. of the germane in THF to a soln. of the Li propionitrile (prepd. from propionitrile and Li diisopropylamide) in THF, stirring at -78°C for 10 min, then at 0°c for 0.5 h, quenching the react. with aq. NH4Cl; sepn. of the org. layer, extn. of the aq. layer (ether), washing the combined extracts (H2O and satd. aq. NaCl), drying (MgSO4), concg., column chromy. (silica gel, hexane-ethyl acetate 20:1-10:1), isomer ratio: 55:45;