反应详情

A mixture of 2-[3-(2-benzothiazolylmethoxy)benzoylamino]-4-[3-(4-chlorophenylsulfonyl)propyl]phenoxyacetic acid (200 mg, 0.31 mmol), methanesulfonamide (31 mg), 4-dimethylaminopyridine (45 mg), 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (125 mg) and dichloromethane (10 ml) was stirred at room temperature for 3 days. The reaction solution was washed with 1 N hydrochloric acid, water and brine in that order, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. By recrystallizing the resulting solid material from acetonitrile (2 ml), 2-[2-[3-(2-benzothiazolylmethoxy)benzoylamino]-4-[3-(4-chlorophenylsulfonyl)propyl]phenoxy]-N-(methanesulfonyl)acetamide 0.5 hydrate (70 mg, 0.096 mmol, 31%) was obtained as colorless crystals.

1. washThe reaction solution was washed with 1 N hydrochloric acid, water and brine in that order
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customBy recrystallizing the resulting solid material from acetonitrile (2 ml)