反応 #1579

反応方程式

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

収率 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

収率 55.9%

溶媒

acetic acid

反応条件

後処理

1. 1
   温度cooled
2. 2
   洗浄The organic mixture is washed sequentially with water, saturated sodium hydrogen carbonate solution and brine
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   濃縮concentrated in vacuo
5. 5
   その他to obtain a yellow semi-solid

実験手順

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.).

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