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Dimethylformamide → 4-Ethoxy-1-fluoro-2-nitrobenzene

HRID 1028222
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HRID 1028222 반응식
CN(C=O)C.[F:6][C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][C:8]=1[N+:14]([O-:16])=[O:15].[H-].[Na+].[CH2:19](I)[CH3:20]>C(OCC)(=O)C>[CH2:19]([O:13][C:10]1[CH:11]=[CH:12][C:7]([F:6])=[C:8]([N+:14]([O-:16])=[O:15])[CH:9]=1)[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 167518614-Fluoro-3-nitrophenol

생성물 1

HCID 567772444-Ethoxy-1-fluoro-2-nitrobenzene수율 93%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

To a DMF (10 mL) solution of 4-fluoro-3-nitro-phenol (628 mg), sodium hydride (purity: 55% or higher, 209 mg) was added in small portions at room temperature. After 30 minutes, ethyl iodide (0.38 mL) was added thereto at room temperature. After 2 hours, the reaction mixture was diluted with ethyl acetate, washed with saturated sodium bicarbonate and saturated brine, then dried over sodium sulfate, and then concentrated. The residue was purified by column chromatography (hexane/ethyl acetate) to obtain the title compound (685 mg, 93%) as a yellow solid.

후처리

  1. customat room temperature
  2. waitAfter 2 hours
  3. washwashed with saturated sodium bicarbonate and saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-b9e548aa4e894a189a0d38bdd6c2b12a
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735425B2

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