反应详情

42 mg of 4-methylbenzenesulphonic acid hydrate are added to a solution of 300 mg of N-(3-fluoro-2-hydroxyphenyl)-2-[4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetamide in 20 ml of xylene. After refluxing for six hours (assembly with Dean-Stark apparatus), the medium is concentrated to dryness under reduced pressure. After purification by silica column chromatography of the solid residue, eluent: gradient of pure CH2Cl2 to CH2Cl2/MeOH: 95/05, the product obtained is taken up with twice 20 ml of diethyl ether and then spin-filter-dried and dried under vacuum. 110 mg of 2-[(7-fluoro-1,3-benzoxazol-2-yl)methyl]-6-(morpholin-4-yl)pyrimidin-4(3H)-one are obtained in the form of a white powder, the characteristics of which are the following:

1. temperatureAfter refluxing for six hours (assembly with Dean-Stark apparatus), the medium
2. concentrationis concentrated to dryness under reduced pressure
3. customAfter purification by silica column chromatography of the solid residue, eluent
4. customgradient of pure CH2Cl2 to CH2Cl2/MeOH: 95/05, the product obtained
5. customspin-filter-dried
6. customdried under vacuum