反応 #1561

反応方程式

Nitric acid

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

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title product

収率 75.6%

1-(2-Chloro-4-fluoro-5-nitrophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

収率 75.6%

溶媒

—

ice water

sulfuric acid

反応条件

後処理

1. 1
   温度while maintaining the reaction mixture temperature below 10° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   温度cooled to 10° C
4. 4
   ろ過The resultant aqueous mixture is filtered
5. 5
   その他to obtain a solid which
6. 6
   洗浄is washed with water
7. 7
   その他air-dried

実験手順

Nitric acid (70% real, 8.3 mL, 0.131 mol) is added to a solution of 1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (32.4 g, 0.119 mol) in concentrated sulfuric acid while maintaining the reaction mixture temperature below 10° C. After the addition is complete, the reaction mixture is stirred at room temperature for 30 minutes, cooled to 10° C and diluted with ice-water. The resultant aqueous mixture is filtered to obtain a solid which is washed with water and air-dried to give the title product as a white solid (28.5 g, mp 135°-139° C.).

出典