Diethyl Ether → HCID 23448078, compound

Participants

Reaction Steps

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.

Provenance & Evidence