反应详情

Sodium (1.031 g) was dissolved in 20.130 g of 1,3-propanediol and 2.091 g of N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide was added thereto with stirring at room temperature. The reaction mixture was stirred at room temperature for 50 minutes and then at 60° C. for 50 minutes and poured into a mixture of 1N hydrochloric acid and ice. This was extracted with ethyl acetate and the ethyl acetate layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo and the resulting residue was purified by a silica gel column chromatography (chloroform-methanol=100:1 to 20:1). The resulting syrup was crystallized in ether and collected by filtration to give 1.817 g of N-[6-(3-hydroxypropyloxy)-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide.

1. stirringThe reaction mixture was stirred at room temperature for 50 minutes
2. extractionThis was extracted with ethyl acetate
3. dry with materialthe ethyl acetate layer was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. customthe resulting residue was purified by a silica gel column chromatography (chloroform-methanol=100:1 to 20:1)
7. customThe resulting syrup was crystallized in ether
8. filtrationcollected by filtration