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Methyl iodide → 5-Bromo-1,2-dimethyl-3-nitrobenzene

HRID 2208700
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HRID 2208700 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7](O)=O.C(=O)([O-])[O-].[Na+].[Na+].CI>CN(C=O)C>[CH3:7][C:6]1[CH:10]=[C:2]([Br:1])[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]=1[CH3:11]
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 137700085-Bromo-2-methyl-3-nitrobenzoic acid

생성물 1

HCID 123818655-Bromo-1,2-dimethyl-3-nitrobenzene수율 99%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

To stirred solution of 5-bromo-2-methyl-3-nitrobenzoic acid, prepared analogously to above, (287 g, 1103 mmol) in DMF (150 mL), sodium carbonate (468 g, 4415 mmol) and methyl iodide (626.6 g, 4415 mmol) were added. Resulting mixture was heated at 60° C. for 8 h. On completion, solid was remove by filtration, and the residue washed with diethyl ether (5 times). The combined organic layers were dried, concentrated under reduced pressure to give methyl 5-bromo-2-methyl-3-nitrobenzene (302 g, 99%).

후처리

  1. customResulting mixture
  2. customOn completion, solid was remove by filtration
  3. washthe residue washed with diethyl ether (5 times)
  4. customThe combined organic layers were dried
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9104854ee5da4a6eb6955f0e39a2cc11
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376422B2

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