反应详情

To a solution of crude 2-{3-[((S)-1-dimethylaminomethyl-2-phenyl-ethylamino)-methyl]-benzyl}-1,1-dioxo-1λ6-isothiazolidine-3-carboxylic acid ethyl ester (360 mg, approx. 0.67 mmol) in tetrahydrofuran (4 mL) was added lithium hydroxide hydrate (57.4 mg, 1.37 mmol) followed by water (1 mL). It was stirred at room temperature for 2 h. To the stirred solution was added ˜15 drops 1N hydrochloric acid to bring the pH to 4.5. The sample was concentrated to dryness and dried over phosphorus pentoxide overnight. The crude 2-{3-[((S)-1-dimethylaminomethyl-2-phenyl-ethylamino)-methyl]-benzyl}-1,1-dioxo-1λ6-isothiazolidine-3-carboxylic acid (350 mg, ca 80% pure) (LiCl present) was used in the next step.

1. concentrationThe sample was concentrated to dryness
2. dry with materialdried over phosphorus pentoxide overnight