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Ethyl Acetate → HCID 58306846, 화합물

HRID 1909864
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HRID 1909864 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:12]=[CH:13][C:14]=1[CH3:15])[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH3:2].[Br:16]N1C(=O)CCC1=O.C(OCC)(=O)C>N(C(C)(C)C#N)=NC(C)(C)C#N.CCCCCC>[Br:16][CH2:15][C:14]1[CH:13]=[CH:12][C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5][C:4]=1[O:3][CH2:1][CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 67184N-bromobutanimideHCID 23136282Ethyl 3-ethoxy-4-methylbenzoate

생성물 1

HCID 58306846HCID 58306846, 화합물수율 87%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 8058Hexane용매

실험 절차

To a mixture of ethyl 3-ethoxy-4-methylbenzoate (2.0 g), N-bromosuccinimide (1.9 g) and ethyl acetate (40 mL) was added 2,2′-azobis(2-methylpropionitrile) (15 mg), followed by stirring for 14 hours under heating with reflux. The mixture was left to be cooled, hexane was added thereto, the precipitated solid was separated by filtration, and the obtained filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane:5/95) to obtain ethyl 4-(bromomethyl)-3-ethoxybenzoate (2.4 g).

후처리

  1. temperatureunder heating
  2. temperaturewith reflux
  3. waitThe mixture was left
  4. temperatureto be cooled
  5. customthe precipitated solid was separated by filtration
  6. concentrationthe obtained filtrate was concentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane:5/95)

출처 및 근거

ORD 기록
ord-f9de10e459c14630af8718dfa6601824
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598355B2

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