Bromine → 1-Bromo-2,4-dimethoxy-5-nitrobenzene

HRID 844296

반응식

HRID 844296 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12].[Br:14]Br.S(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[Br:14][C:6]1[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[O:9][CH3:10]

참가 물질

5

반응물 3

HCID 24408Bromine2회HCID 786332,4-Dimethoxy-1-nitrobenzeneHCID 23665763Sodium Bisulfite

생성물 1

HCID 185436101-Bromo-2,4-dimethoxy-5-nitrobenzene

시약·촉매·용매 1

HCID 6212Chloroform용매3회

실험 절차

To a solution of 2,4-dimethoxy-nitrobenzene (0.50 g) in chloroform (3 mL) is added dropwise a solution of bromine (0.23 g) in chloroform (1 mL) and the mixture is allowed to stir at room temperature for approximately 15 hours. Additional bromine (0.15 g) in chloroform (1 mL) is added and the reaction is stirred for an additional 4 hours. The mixture is then poured onto 5% aqueous sodium bisulfite and then extracted with chloroform. Pooled organic extracts are then washed successively with 5% aqueous sodium bisulfite then saturated sodium chloride, and then dried over anhydrous sodium sulfate. Removal of the solvent under reduced pressure and recrystallization of the residue from toluene provides the desired product as a yellow solid.

후처리

  1. stirringthe reaction is stirred for an additional 4 hours
  2. extractionextracted with chloroform
  3. washPooled organic extracts are then washed successively with 5% aqueous sodium bisulfite
  4. dry with materialsaturated sodium chloride, and then dried over anhydrous sodium sulfate
  5. customRemoval of the solvent
  6. customunder reduced pressure and recrystallization of the residue from toluene

출처 및 근거

ORD 기록
ord-fac832a8573a4e2b99a8993e190f8d4d
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380243B1

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