반응 #1579

반응 방정식

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

3,4,5,6-tetrahydrophthalic anhydride

ethyl acetate

→

title product

수율 55.9%

N-{4-Chloro-2-fluoro-5-[hexahydro-2,4,6-trioxo-3-(2-propynyl)-s-triazin-1-yl]phenyl}-1-cyclohexene-1,2-dicarboximide

수율 55.9%

용매

acetic acid

반응 조건

후처리

1. 1
   온도cooled
2. 2
   세척The organic mixture is washed sequentially with water, saturated sodium hydrogen carbonate solution and brine
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   농축concentrated in vacuo
5. 5
   기타to obtain a yellow semi-solid

실험 절차

A solution of 1-(5-amino-2-chloro-4-fluorophenyl)-3-(2-propynyl)-s-triazine-2,4,6-(1H,3H,5H)-trione (1.50 g, 4.83 mmol), and 3,4,5,6-tetrahydrophthalic anhydride (0.73 g, 4.83 mmol) in acetic acid (3 mL) is heated at 100° C. for 5 hours, cooled, and poured into ethyl acetate, The organic mixture is washed sequentially with water, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a yellow semi-solid. Flash column chromatography of the semi-solid using silica gel and an ethyl acetate/hexanes (1:2) solution gives the title product as a white solid (1.20 g, mp 127°-135° C.).

출처