Potassium Carbonate → HCID 69948095, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 11-(2-bromoethylidene)-2-chloro-6,11-dihydrodibenzo[b,e]thiepine (1.76 g, 0.005 mol, prepared as described in Example 3) in N,N-dimethylformamide (20 ml), potassium carbonate (2.33, 0.006 mol) and 4-piperidinecarboxylic acid ethyl ester (0.86 g, 0.0055 mol) were added and the mixture was stirred at 50° C. for 3 h. The reaction mixture was diluted with dichloromethane (80 ml), the solid was filtered off and the filtrate was washed with water (4×30 ml). The dichloromethane solution was dried (MgSO4) and the solvent removed in vacuo. The oily residue (2.34 g) was dissolved in acetone and treated with an ethanolic solution of oxalic acid. The precipitated crude hydrogen oxalate salt (5.8 g) was recrystalised from aqueous ethanol, to give 1.12 g (87%) of 1-(2-(2-chloro-6,11-dihydrodibenzo[b,e]thiepin-11-ylidene)-1-ethyl)-4-piperidinecarboxylic acid ethyl ester hydrogen oxalate.

Provenance & Evidence