反应详情

温度

75 °C

To a solution of 1-(2-pyridyl)-2-thiourea (765 mg, 5.0 mmol) in acetone (14 mL) was added slowly 2-bromo-3-hydroxypropenal (755 mg, 5.0 mmol, for preparation see J. Org. Chem. 28, 3243, 1963) in acetone (14 mL) over a period of 5 min. After stirring for 1.5 h, a precipitate formed. The solids were separated, washed with acetone (10 mL) and then taken into mixed solvent (ethanol/water=1/1, 9 mL). To this suspension was added sodium acetate (1.23 g, 15.0 mmol) and the resulting mixture was heated at 75° C. for 1 h. After cooling to RT, the mixture was filtered and the solids were washed with water (10 mL), and dried in vacuo to provide compound A, 2-(pyridin-2-ylamino)-thiazole-5-carbaldehyde (533 mg, 52%) as a solid. LC/MS; (M+H)+=206

1. customa precipitate formed
2. customThe solids were separated
3. washwashed with acetone (10 mL)
4. additioninto mixed solvent (ethanol/water=1/1, 9 mL)
5. temperatureAfter cooling to RT
6. filtrationthe mixture was filtered
7. washthe solids were washed with water (10 mL)
8. customdried in vacuo