反応 #4331

反応方程式

acetic acid

sodium nitrite

2,5-difluoro-N-benzenesulphonylaniline

nitric acid

→

2,5-difluoro-4-nitro-N-benzenesulphonylaniline

溶媒

water

water

反応条件

後処理

1. 1
   workup.ADDITIONare added
2. 2
   温度After cooling it
3. 3
   その他The expected product precipitates
4. 4
   ろ過After being filtered off
5. 5
   洗浄washed
6. 6
   その他is recrystallized from 250 ml of acetic acid

実験手順

To 310 ml of acetic acid diluted with 160 ml of water are added: 1.5 g of sodium nitrite, 0.16 mole (42 g) of 2,5-difluoro-N-benzenesulphonylaniline prepared in the previous stage and 0.94 mole (39 ml) of nitric acid (d=1.52). The reaction mixture is heated to 96° C. for 1 hour. After cooling it is poured onto 1 kg of ice and water. The expected product precipitates. After being filtered off and washed to neutrality it is recrystallized from 250 ml of acetic acid; it melts at 176° C.

出典