반응 #325875

반응 방정식

sulfuric acid

Sodium nitrate

2-Bromo-phenol

→

2-bromo-6-nitro-phenol

수율 42.8%

용매

water

ethyl acetate

반응 조건

후처리

1. 1
   기타was kept below 25° C
2. 2
   세척The mixture was washed with water and saturated brine
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   여과filtered
5. 5
   농축the filtrate was concentrated under reduced pressure
6. 6
   기타The resulting residue was purified by silica gel column chromatography

실험 절차

A solution of 60 mL of concentrated sulfuric acid diluted with 186 mL of water was cooled to room temperature. Sodium nitrate (79.2 g, 0.93 mol) was added to the solution. 2-Bromo-phenol 1a (60 mL, 0.52 mol) was added dropwise at such a rate that the reaction temperature was kept below 25° C. The reaction mixture was stirred at room temperature for 2 hours. The precipitate was dissolved in 320 mL of ethyl acetate. The mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound 2-bromo-6-nitro-phenol 1b (48.2 g, yield 42.8%) as a yellow solid.

출처