반응 #802275

반응 방정식

1-bromo-4-fluoro-2-methyl-5-nitrobenzene

hydrogen

hydrogen

→

title compound

수율 63.2%

5-bromo-2-fluoro-4-methylaniline

수율 63.2%

용매

ethanol

반응 조건

후처리

1. 1
   기타De-pressurize the reaction vessel, remove the catalyst
2. 2
   여과by filtration
3. 3
   기타evaporate the filtrate to dryness
4. 4
   여과Add MTBE, then filter again
5. 5
   기타evaporate the filtrate
6. 6
   기타Collect the solids
7. 7
   여과by filtration
8. 8
   세척wash with cold hexanes
9. 9
   기타dry in vacuo

실험 절차

Combine crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (32.4 g, 138 mmol), ethanol (100 mL) and Raney Nickel (1.00 g, 17.04 mmol) in a shaker flask. Charge the flask with hydrogen (275 kPa) and agitate until the absorption of hydrogen ceases. De-pressurize the reaction vessel, remove the catalyst by filtration, and evaporate the filtrate to dryness. Add MTBE, then filter again and evaporate the filtrate. Stir residue in hexanes. Collect the solids by filtration, wash with cold hexanes and dry in vacuo to provide the title compound (17.8 g, 63%) as a dark solid. MS (m/z): 204.0 (M+H+)/206.0 (M+H+).

출처