反应详情

Sodium (230 mg) was dissolved in 5.6 ml of ethylene glycol and 495 mg of N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide was added thereto under ice cooling with stirring. The reaction mixture was stirred at 80° C. for three hours and poured into a mixture of 1N hydrochloric acid and ice. The crystals separated out therefrom were collected by filtration and the resulting crystals were purified by a silica gel column chromatography (chloroform-methanol=20:1) to give 500 mg of N-[6-(2-hydroxyethoxy)-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide.

1. stirringThe reaction mixture was stirred at 80° C. for three hours
2. customThe crystals separated out
3. filtrationtherefrom were collected by filtration
4. customthe resulting crystals were purified by a silica gel column chromatography (chloroform-methanol=20:1)