反应 #1328450

反应方程式

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

收率 83.3%

溶剂

N,N-dimethylformamide

反应条件

后处理

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
   萃取the mixture was extracted with ethyl acetate
5. 5
   洗涤The organic layer was washed with saturated aqueous sodium chloride solution
6. 6
   干燥dried over anhydrous magnesium sulfate
7. 7
   浓缩concentrated

实验过程

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).

来源