C(N(CC)CC)C.[O:8]=[C:9]([N:12]([C:28](=[O:31])[CH2:29][CH3:30])[C:13]1[C:18]([C:19]2[S:20][CH:21]=[CH:22][CH:23]=2)=[CH:17][CH:16]=[CH:15][C:14]=1[S:24](O)(=[O:26])=[O:25])[CH2:10][CH3:11].P(Cl)(Cl)(Cl)(Cl)[Cl:33].CCOCC>ClCCl>[O:8]=[C:9]([N:12]([C:28](=[O:31])[CH2:29][CH3:30])[C:13]1[C:18]([C:19]2[S:20][CH:21]=[CH:22][CH:23]=2)=[CH:17][CH:16]=[CH:15][C:14]=1[S:24]([Cl:33])(=[O:26])=[O:25])[CH2:10][CH3:11]To a solution of 2.8 g (6.1 mmol) of the N,N-diethylethanamine salt of 2-[bis(1-oxopropyl)amino]-3-thien-2-ylbenzenesulphonic acid in 6 ml of dichloromethane are added, at 0° C., 1.3 g (6.1 mmol) of phosphorus pentachloride and the reaction mixture is allowed to warm to room temperature. The mixture is then heated for 5 hours at the reflux temperature and then allowed to cool to room temperature. Ether is added, the mixture is filtered and the residue is precipitated from an ether/pentane mixture (1/1). The mixture is filtered and the filtrate is concentrated under reduced pressure and purified by chromatography on a column of florisil™. 2.2 g of product are obtained, which product is crystallized from an ether/pentane mixture.
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