反应详情

This compound may be obtained in the following way: a mixture of 10 g 4-hydroxy-6-methylthio-pyrimido[5,4-d]pyrimidine, 16 ml hexamethyldisilazane, 32.5 g 3-chloro-4-fluoro-aniline and 1 g p-toluenesulphonic acid hydrate are heated at boiling point for 12 hours. Then 500 ml methanol is added and the mixture heated at boiling point for a further hour. The solvents are distilled off in a rotary evaporator, the residue is dissolved in methylene chloride, the solution is extracted with 100 ml 2N sodium hydroxide and dried over magnesium sulfate. After distilling off the solvent in a rotary evaporator the residue is triturated with 200 ml ether, filtered off and washed several times with ether.

1. customThis compound may be obtained in the following way
2. temperatureare heated
3. customfor 12 hours
4. temperaturethe mixture heated
5. distillationThe solvents are distilled off in a rotary evaporator
6. dissolutionthe residue is dissolved in methylene chloride
7. extractionthe solution is extracted with 100 ml 2N sodium hydroxide
8. dry with materialdried over magnesium sulfate
9. distillationAfter distilling off the solvent
10. customin a rotary evaporator the residue
11. customis triturated with 200 ml ether
12. filtrationfiltered off
13. washwashed several times with ether