반응 #1565

반응 방정식

water

1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

potassium carbonate

isopropyl bromoacetate

→

title product

수율 92.4%

Isopropyl 3-(2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate

수율 92.4%

용매

methylene chloride

ether

N,N-dimethylformamide

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   추출The organic extract
3. 3
   세척is washed sequentially with water and brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated in vacuo
6. 6
   기타to obtain an oil

실험 절차

A mixture of 1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (40.9 g, 0.150 mol), potassium carbonate (31.1 g, 0.225 mol) and isopropyl bromoacetate (29.1 mL, 0.225 mol) in N,N-dimethylformamide is stirred at room temperature for 2 hours, poured into water and extracted with ethyl acetate. The organic extract is washed sequentially with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain an oil. Flash column chromatography of the oil using silica gel and 0% to 10% ether in methylene chloride solutions gives the title product as a white solid (51.5 g, mp 127°-128° C.).

출처