반응 #533402

반응 방정식

iodine

4-methyl-3-nitro-benzoic acid

→

3-iodo-4-methyl-5-nitro-benzoic acid

수율 95.0%

용매

sulfuric acid

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   workup.ADDITIONpoured over ice
3. 3
   기타The mixture was partitioned between ethyl acetate and aqueous sodium bisulfite
4. 4
   기타the organic layer was separated
5. 5
   건조dried over MgSO4
6. 6
   여과filtered
7. 7
   농축concentrated under reduced pressure

실험 절차

To a mixture of iodine (19.6 g, 77.3 mmol) in fuming sulfuric acid (35 mL) was added 4-methyl-3-nitro-benzoic acid (10.0 g, 55.2 mmol). The mixture was stirred at 85° C. over night, then cooled to room temperature and poured over ice. The mixture was partitioned between ethyl acetate and aqueous sodium bisulfite, and the organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to give 16.06 g (95%) of 3-iodo-4-methyl-5-nitro-benzoic acid.

출처