反应详情

0.2 ml (2.32 mmol) of 30% strength hydrogen peroxide solution was added to a solution of 96 mg (0.2 mmol) of 5-chloro-2-methoxy-N-(2-(1-(3-cyclopropylthioureidosulfonyl)piperidin-4-yl)ethyl)benzamide in 2 ml of 0.5 M sodium hydroxide solution at 0° C. After the reaction mixture had been kept at 0° C. for 1 hour, 200 mg of sodium sulfite were added, and the mixture was acidified by means of 2 M hydrochloric acid. The precipitated solid was filtered off, washed with water until neutral and purified by chromatography (silica gel; toluene/ethanol/ethyl acetate 8/1/1). The crude product was crystallized from methanol. 30 mg (32%) of the title compound were obtained as a colorless solid.

1. filtrationThe precipitated solid was filtered off
2. washwashed with water until neutral and
3. custompurified by chromatography (silica gel; toluene/ethanol/ethyl acetate 8/1/1)
4. customThe crude product was crystallized from methanol