Triethylamine → HCID 68908400, Verbindung

Reaktionsgleichung

[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4].C(N(CC)CC)C.Cl[P:23]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O1CCCC1>[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:12])=[O:13])=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4].[C:30]1([PH:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

Komponenten

Versuchsvorschrift

Commercially available 4-butylbenzene-1-sulfonamide (9.376 mole, 1 eq) was dissolved in tetrahydrofuran (20 mL) and triethylamine (25 mmole), leading to a clear colorless solution. Distilled chlorobisphenylphosphine (9.376 mmole, 1.0 eq) was added dropwise under strong magnetic stirring at room temperature. The suspension was left to stir overnight at room temperature. The suspension was then filtered under argon atmosphere and the resulting clear solution was evaporated to a white solid. The product was redissolved in 10 mL of diethylether leading to a clear solution. 10 mL of pentane were added dropwise to the solution causing a white solid to crash out. The organic layer was syringed out, and the white solid obtained was washed twice with 10 mL of pentane. The product was filtered over a short silica gel column with dichloromethane as eluent. The product was obtained as white solid. The product was characterized by 1H, 31P, 13C NMR.