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

HRID 2208910
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인쇄 미리보기

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HRID 2208910 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 119.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

To a stirred solution of 5-bromo-2-methyl-3-nitrobenzoic acid (287 g, 1100 mmol) in DMF (150 mL), were added sodium carbonate (468 g, 4415 mmol) and methyl iodide (627 g, 4415 mmol). The mixture was heated at 60° C. for 8 h. The precipitate was filtered and washed with diethyl ether (5 times). The combined organic layers were dried, concentrated under reduced pressure giving the title compound (302 g, 99%) which was used directly without further purification.

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with diethyl ether (5 times)
  3. customThe combined organic layers were dried
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1b8b8c030ea543b8b0eb36058fca9760
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376422B2

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