反应详情

温度

95 °C

To a stirred solution of hydroxylamine hydrochloride (10.0 g, 143.0 mmol) and sodium acetate trihydrate (20.0 g, 146.9 mmol) in water (100 ml) at 30° C. was added a hot solution of 4-[2-[2-ethyl-4-methyl-6-oxo-1,6-dihydro-1-pyrimidinyl]ethoxy]benzaldehyde (5.72 g, 20.0 mmol) (obtained from preparation 3) in ethanol (100 ml). The reaction mixture was immersed in a preheated oil bath (95° C.) and refluxed for 3 h. The reaction mixture was then cooled to room temperature and concentrated to a volume where crystals of oxime started separating out and the mixture was kept aside for 30 min. to 1 h at 25° C. The resultant crystals were filtered and washed with water and dried to obtain the title compound (5.42 g, 90%).

1. customThe reaction mixture was immersed in a preheated oil bath
2. temperatureThe reaction mixture was then cooled to room temperature
3. concentrationconcentrated to a volume where crystals of oxime
4. customstarted separating out and the mixture
5. waitwas kept aside for 30 min. to 1 h at 25° C
6. filtrationThe resultant crystals were filtered
7. washwashed with water
8. customdried