反応 #1565

反応方程式

water

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

potassium carbonate

isopropyl bromoacetate

→

title product

収率 92.4%

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

収率 92.4%

溶媒

methylene chloride

ether

N,N-dimethylformamide

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   抽出The organic extract
3. 3
   洗浄is washed sequentially with water and brine
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated in vacuo
6. 6
   その他to obtain an oil

実験手順

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.).

出典