Ethanol → HCID 10074926, compound

Participants

Reaction Steps

773 mg of (±)-cis-5-(2-dimethylaminoethyl)-2,3- dihydro-3-hydroxy-2-(4-methoxyphenyl)-8-phenoxy-1 5- benzothiazepin-4(5H)-one (prepared as described in Example 1) were dissolved in 5 ml of pyridine, and 1 ml of acetic anhydride was added at room temperature to the resulting solution. The mixture was then left to stand for 14 hours. At the end of this time, 2 ml of ethanol were added to the reaction mixture, and after the mixture had been left to stand for 30 minutes, 30 ml of ethyl acetate were added. The mixture was then washed with an aqueous solution of sodium bicarbonate and with an aqueous solution of sodium chloride in that order, after which it was dried over anhydrous magnesium sulfate, and concentrated by evaporation under reduced pressure to obtain a concentrate. This concentrate was purified by chromatography through a silica gel column, using a 20 : 1 by volume mixture of methylene chloride and methanol as the eluent, to give the title compound as a solid.

Provenance & Evidence