反应详情

Sodium metal (276 mg, 12 mmol) was added portion wise to ethanol (15 ml) under a nitrogen atmosphere and the mixture allowed to stir at room temperature for 30 minutes until the reaction became homogeneous. 4-Chloro-benzamidine (hydroiodide salt) (1.41 g, 5 mmol) was then added in one portion and the reaction stirred at room temperature for a further 60 minutes. 2-Methyl-3-oxo-propionic acid ethyl ester (716 mg, 5.5 mmol) was finally added drop wise. The reaction was left to stir at room temperature overnight before quenching the reaction slowly with 2M Hydrochloric acid until reaction pH measured pH 1. The resulting precipitate was filtered and air dried, to give 2-(4-Chloro-phenyl)-5-methyl-3H-pyrimidin-4-one as a white solid (570 mg, 2.58 mmol, 52% yield).

1. stirringthe reaction stirred at room temperature for a further 60 minutes
2. waitThe reaction was left
3. stirringto stir at room temperature overnight
4. custombefore quenching
5. customthe reaction slowly with 2M Hydrochloric acid
6. customuntil reaction pH measured pH 1
7. filtrationThe resulting precipitate was filtered
8. customair dried