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Methyl iodide → 1-Bromo-5-fluoro-4-methoxy-2-nitrobenzene

HRID 639010
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HRID 639010 반응식
[Br:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([OH:11])=[C:4]([F:12])[CH:3]=1.[C:13](=O)([O-])[O-].[K+].[K+].CI>CN(C=O)C>[CH3:13][O:11][C:5]1[CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]([Br:1])=[CH:3][C:4]=1[F:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 179763164-Bromo-2-fluoro-5-nitrophenol

생성물 1

HCID 179763101-Bromo-5-fluoro-4-methoxy-2-nitrobenzene수율 97%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 4-bromo-2-fluoro-5-nitrophenol (25 g, 106 mmol) in DMF (200 mL) was treated with potassium carbonate (28.9 g, 212 mmol) and methyl iodide (12.8 mL, 212 mmol). The reaction mixture was stirred at 60 C for 5 hours and evaporated in vacuo. The mixture was partitioned between water and ethyl acetate. The organic layer was dried over magnesium sulfate and evaporated under vacuum to afford the product (25.6 g, 97%) as a yellow solid. LC-MS (ES) (M+H)+ m/z=251.

후처리

  1. customevaporated in vacuo
  2. customThe mixture was partitioned between water and ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-0a3df1d3f7944ced89caa6387a12a789
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691850B2

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