反应 #4999

反应方程式

potassium carbonate

methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate

methoxyamine hydrochloride

water

→

aimed compound

收率 60.0%

methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-[1-(N-methoxyimino)ethyl]benzoate

收率 60.0%

溶剂

methanol

反应条件

后处理

1. 1
   温度the resultant liquor was heat-refluxed for 3 hours
2. 2
   其他an oily product thus precipitated
3. 3
   萃取was extracted with ethyl acetate
4. 4
   洗涤The ethyl acetate layer was washed with water
5. 5
   其他was dried
6. 6
   workup.DISTILLATIONto distill off ethyl acetate under reduced pressure
7. 7
   其他The residue thus obtained
8. 8
   其他was purified by chromatography

实验过程

1.0 g of methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate and 0.5 g of methoxyamine hydrochloride were dissolved in 6 ml of methanol, and the resultant solution was refluxed for 15 minutes. After cooling the mixed liquor to room temperature, 0.8 g of potassium carbonate was added to this liquor and the resultant liquor was heat-refluxed for 3 hours. The reaction liquor was poured into a large amount of water, and an oily product thus precipitated was extracted with ethyl acetate. The ethyl acetate layer was washed with water, and was dried to distill off ethyl acetate under reduced pressure. The residue thus obtained was purified by chromatography to obtain 0.65 g of the aimed compound (refractive index=1.5709) at a yield of 59%.

来源