반응 #82663

반응 방정식

3-chloro-2,4-difluoro-6-nitro-(trifluoroacetamido)benzene

→

crystalline yellow solid

수율 6.9%

3-Chloro-2,4-difluoro-6-nitroaniline

수율 6.9%

용매

K2CO3 methanol water

반응 조건

후처리

1. 1
   기타The solution was evaporated
2. 2
   기타to remove the methanol
3. 3
   여과was filtered
4. 4
   세척washed by water
5. 5
   기타dried

실험 절차

A solution of 6.35 g (20.8 mmol) of 3-chloro-2,4-difluoro-6-nitro-(trifluoroacetamido)benzene in 60 mL of 7% K2CO3 methanol/water (3:2) was stirred at 25° C. for 4 h. The solution was evaporated to remove the methanol. Solid was observed in the residue and it was filtered and washed by water, and dried to leave 301 mg of crystalline yellow solid, mp 96°-97° C. 1H NMR (CDCl3), 6.07 (mb, 2), 7.815 (dd, 1, J=1.92, 9.13). More solid was observed after the mother aqueous solution was allowed to stand at room temperature overnight. It was filtered and washed by water, and dried to leave yellow solid (1.01 g). More solid was crystallized from the mother solution. It was collected three more times to leave 2.48 g of a yellow solid. 1H NMR is identical with above, total yield 3.80 g (87%).

출처