反应详情

In 7 ml of tetrahydrofuran was dissolved 0.70 g of diphenylmethyl [4-(3-aminopropyl)-2,3-dioxopiperazin-1-yl]acetate hydrochloride, and 0.36 g of 4-cyanobenzenesulfonyl chloride and then 0.58 ml of triethylamine were added thereto under ice-cooling. After stirring at room temperature for 30 minutes, the reaction mixture was added to a mixed solvent of 20 ml of ethyl acetate and 20 ml of water and the pH was adjusted to 3 with 2N hydrochloric acid. The organic layer was separated, washed with water and then a saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent; chloroform : methanol=20:1) to obtain 0.43 g of diphenylmethyl [4-[3-(4-cyanobenzenesulfonyl-amino)propyl]-2,3-dioxopiperazin-1-yl]acetate as a yellow foamy substance.

1. temperatureunder ice-cooling
2. customThe organic layer was separated
3. washwashed with water
4. dry with materiala saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customthe resulting residue was purified by a silica gel column chromatography (eluent; chloroform : methanol=20:1)