反应 #1528394

反应方程式

2,5-difluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene

sodium hydride

2-benzyloxyphenol

→

2-(2-benzyloxyphenoxy)-5-fluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene

收率 80.0%

溶剂

N,N-dimethylformamide

N,N-dimethylformamide

N,N-dimethylformamide

反应条件

后处理

1. 1
   workup.ADDITIONwas added dropwise at the same temperature
2. 2
   workup.STIRRINGthe mixture was stirred for 1 hour
3. 3
   萃取extracted with ethyl acetate
4. 4
   洗涤The organic layer was washed successively once with 1N—HCl and once with saturated aqueous sodium chloride solution
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   浓缩concentrated

实验过程

A mixture of 4.05 g of 2-benzyloxyphenol and 9.5 ml of N,N-dimethylformamide was added dropwise to a mixture of 0.80 g of sodium hydride and 20 ml of N,N-dimethylformamide under ice cooling and the mixture was stirred for 30 minutes. A mixture of 7.1 g of 2,5-difluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene and 17 ml of N,N-dimethylformamide was added dropwise at the same temperature and the mixture was stirred for 1 hour. The reaction solution was poured into ice-water and extracted with ethyl acetate. The organic layer was washed successively once with 1N—HCl and once with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica-gel column chromatography to give 8.6 g of 2-(2-benzyloxyphenoxy)-5-fluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene.

来源