反应详情

2-Chloro-5-bromopyrimidine (10 mmol) was added to a solution of pyrimidine-2-thione (10 mmol) in ethanolic 0.24 M NaOEt (45 ml), the mixture heated under reflux for 2 hours, the solvent distilled off, the residue extracted with chloroform (70 ml), the chloroform solution shaken with 2 M NaOH and with water, the dried (MgSO4) solution evaporated and the residue repeatedly extracted with pet. ether leaving the title compound. Yield 35%, m.p. 178°-180° C. (iPrOH). 1H NMR (CDCl3): δ7.13 (H-5'), 8.60 (H-4', H-6'), 8.66 (H-4, H-6).

1. temperaturethe mixture heated
2. temperatureunder reflux for 2 hours
3. distillationthe solvent distilled off
4. extractionthe residue extracted with chloroform (70 ml)
5. dry with materialthe dried (MgSO4) solution
6. customevaporated
7. extractionthe residue repeatedly extracted with pet. ether leaving the title compound