反应详情

A mixture of 160 g (0.65 mol) of N-(6-hydroxy-4-methylpyrimidin-2-yl)-o-nitroaniline, 2 ml of N,N-dimethylformamide and 120 ml of phosphorus oxychloride are heated at reflux for 3 hours. After having been cooled, and black slurry is dissolved in chloroform and this solution is added dropwise to 1 l of water. The temperature is maintained at 35° by the addition of ice. After 1 hour the organic phase is separated off and the aqueous phase is washed with chloroform. The two chloroform solutions are together dried and concentrated by evaporation. The black residue is dissolved in hot toluene, filtered and crystallised by the addition of hexane. 104.9 g (61%) of the title compound of formula ##STR16## (compound No. 2.007) are obtained in the form of crystals having a melting point of 175° C.

1. temperatureare heated
2. temperatureat reflux for 3 hours
3. temperatureAfter having been cooled
4. temperatureThe temperature is maintained at 35° by the addition of ice
5. customAfter 1 hour the organic phase is separated off
6. washthe aqueous phase is washed with chloroform
7. dry with materialThe two chloroform solutions are together dried
8. concentrationconcentrated by evaporation
9. dissolutionThe black residue is dissolved in hot toluene
10. filtrationfiltered
11. customcrystallised by the addition of hexane
12. custom2.007) are obtained in the form of crystals