Hydrochloride methanol → 1-[2-(Methyl{6-[(4-methyl-5-{methyl[2-(methylamino)ethyl]carbamoyl}thiophen-2-yl)amino]hexanoyl}amino)ethyl]piperidin-4-yl biphenyl-2-ylcarbamate

Participants

Reaction Steps

The compound (153 mg, 0.201 mmol) obtained in Example 89d was dissolved in 2 N hydrochloric acid-methanol (2.01 mL, 4.01 mmol), and the mixture was stirred at room temperature for 2 hours. Toluene was added to the reaction mixture, the solvent was evaporated under reduced pressure, the resulting residue was dissolved in ethyl acetate, and the mixture was adjusted to pH 10 with a 1 N aqueous sodium hydroxide solution. The mixture was extracted with ethyl acetate (×2) and dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=100:0→methylene chloride:methanol=10:1, v/v) to give the title compound (122 mg; yield, 92%) as a white solid.

Provenance & Evidence