반응 #82674

반응 방정식

NaNO2

NaI

2-amino-5-nitrobenzotrifluoride

H2SO4

→

solid

수율 94.6%

4-Iodo-3-trifluoromethyl-nitrobenzene

수율 94.6%

용매

H2O

H2O

반응 조건

후처리

1. 1
   workup.STIRRINGThe resulting yellow solution was stirred in an ice-bath for 1 h
2. 2
   workup.ADDITIONit was added dropwise into a well
3. 3
   온도cooled in an ice bath
4. 4
   workup.STIRRINGThe mixture was stirred overnight at 25° C.
5. 5
   여과filtered
6. 6
   세척washed by water
7. 7
   기타dried

실험 절차

To a mixture of 3.1 g (15.0 mmol) of 2-amino-5-nitrobenzotrifluoride in 60 mL of 40% (v/v) H2SO4 stirred in an ice-bath was added dropwise a solution of 2.1 g (30.4 mmol) of NaNO2 in 10 mL of H2O. The resulting yellow solution was stirred in an ice-bath for 1 h and it was added dropwise into a well stirred solution of 10 g of NaI in 250 mL of H2O cooled in an ice bath. Gas releasing and precipitate was observed. The mixture was stirred overnight at 25° C., filtered and washed by water, and dried to leave pale yellow solid (4.5 g, 94%), mp 81°-82° C. 1H NMR (CDCl3), 8.047 (dd, 1), 8.272 (d, 1), 8.483 (d, 1).

출처