反応 #1328451

反応方程式

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

potassium carbonate

sodium chloride

t-butyl chloroacetate

→

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

溶媒

N,N-dimethylformamide

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe mixture was stirred at 40° C. to 60° C. for 2 hours
3. 3
   workup.WAITAfter left
4. 4
   温度for cooling
5. 5
   その他the mixture was subjected to phase separation
6. 6
   洗浄The organic layer was washed with saturated aqueous sodium chloride solution
7. 7
   乾燥dried over magnesium sulfate
8. 8
   濃縮concentrated

実験手順

First, 0.20 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 2 ml of N,N-dimethylformamide, to which 0.083 g of potassium carbonate was added, and the mixture was stirred at room temperature for 50 minutes. Then, 0.077 g of t-butyl chloroacetate was added, and the mixture was stirred at 40° C. to 60° C. for 2 hours. After left for cooling, ice water was poured into the reaction mixture, and after addition of ethyl acetate and saturated aqueous sodium chloride solution, the mixture was subjected to phase separation. The organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography (eluent: n-hexane/ethyl acetate=6/1) to give 10.39 g of t-butyl [2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]acetate (compound a-121).

出典