反応 #1328450

反応方程式

methyl 2-bromopropionate

2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenol

potassium carbonate

→

methyl 2-[2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]propionate

収率 83.3%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe mixture was stirred at 80° C. for 3 hours
3. 3
   温度The reaction mixture was cooled to room temperature
4. 4
   抽出the mixture was extracted with ethyl acetate
5. 5
   洗浄The organic layer was washed with saturated aqueous sodium chloride solution
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   濃縮concentrated

実験手順

First, 0.23 g of 2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenol was dissolved in 6 ml of N,N-dimethylformamide, to which 0.22 g of potassium carbonate was added and 0.13 g of methyl 2-bromopropionate was added under stirring at room temperature, and the mixture was stirred at 80° C. for 3 hours. The reaction mixture was cooled to room temperature and then poured into ice water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.23 g of methyl 2-[2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]propionate (compound b-5).

出典