反应详情

温度

100 °C

A mixture of Compound A (150 mg), 2-chloropyrimidine (61 mg), potassium carbonate (122 mg) and dimethylacetamide (1.5 ml) is heated with stirring at 100° C. for three days. The reaction solution is diluted with aqueous ammonium chloride solution, and extracted with ethyl acetate. The extract is washed and dried. The solvent is evaporated to remove the solvent, and the residue is purified by silica gel column chromatography (solvent; chloroform/methanol =100:1) and further recrystallized from ethyl acetate/n-hexane to give 4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(2-pyrimidinylamino)ethoxy}-pyrimidin-4-yl]benzenesulfonamide hydrate (135 mg) as crystals.

1. temperatureis heated
2. extractionextracted with ethyl acetate
3. washThe extract is washed
4. customdried
5. customThe solvent is evaporated
6. customto remove the solvent
7. customthe residue is purified by silica gel column chromatography (solvent; chloroform/methanol =100:1)
8. customfurther recrystallized from ethyl acetate/n-hexane