反应 #2298640

反应方程式

hydroxylamine hydrochloride

sodium acetate trihydrate

4-[2-[2-ethyl-4-methyl-6-oxo-1,6-dihydro-1-pyrimidinyl]ethoxy]benzaldehyde

→

title compound

收率 90.0%

4-[2-[2-Ethyl-4-methyl-6-oxo-1,6-dihydro-1-pyrimidinyl]ethoxy]benzaldehyde oxime

收率 90.0%

溶剂

water

ethanol

反应条件

后处理

1. 1
   其他The reaction mixture was immersed in a preheated oil bath
2. 2
   温度The reaction mixture was then cooled to room temperature
3. 3
   浓缩concentrated to a volume where crystals of oxime
4. 4
   其他started separating out and the mixture
5. 5
   workup.WAITwas kept aside for 30 min. to 1 h at 25° C
6. 6
   过滤The resultant crystals were filtered
7. 7
   洗涤washed with water
8. 8
   其他dried

实验过程

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%).

来源