反応 #1810797

反応方程式

2,4,5-trifluoronitrobenzene

3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydro pyrimidine

potassium carbonate

→

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

収率 43.0%

溶媒

dimethylsulfoxide

反応条件

後処理

1. 1
   温度The reaction solution was cooled to room temperature
2. 2
   抽出extracted with ethyl acetate
3. 3
   洗浄The organic layer was washed with saturated aqueous sodium chloride solution
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated

実験手順

Into 10 ml of dimethylsulfoxide was dissolved 1.77 g of 2,4,5-trifluoronitrobenzene and 1.94 g of 3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydro pyrimidine. After adding 1.52 g of anhydrous potassium carbonate at room temperature, the mixture was stirred at 80° C. for 1 hour. The reaction solution was cooled to room temperature, and then the solution was poured into ice-water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica-gel column chromatography to give 1.51 g of 2,5-difluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene.

出典