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Potassium Iodide → Methyl 2-acetyl-5-phenylpentanoate

HRID 1368290
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인쇄 미리보기

반응식

HRID 1368290 반응식
[CH3:1][O:2][C:3](=[O:8])/[CH:4]=[C:5](/[O-:7])\[CH3:6].[Na+].[I-].[K+].Br[CH2:13][CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CN1CCCN(C)C1=O>[CH3:1][O:2][C:3](=[O:8])[CH:4]([C:5](=[O:7])[CH3:6])[CH2:13][CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 12503(3-Bromopropyl)benzeneHCID 23681258sodium (2E)-4-methoxy4-oxo-2-buten-2-olate

생성물 1

HCID 11333780Methyl 2-acetyl-5-phenylpentanoate

시약·촉매·용매 1

HCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-용매

반응 조건

온도
80 °C

실험 절차

85 g (616 mmol) of sodium (2E)-4-methoxy-4-oxo-2-buten-2-olate suspended in 1,3-dimethyltetrahydro-2(1H)-pyrimidone and 3.50 g (21.1 mmol) of potassium iodide are treated dropwise with 129 g (646 mmol) of 1-bromo-3-phenylpropane and the mixture is stirred under reflux at 80° C. for 1 h. The cooled mixture is then added to ice water and extracted with diethyl ether. The ether phase is washed with sodium thiosulphate solution, dried, concentrated and chromatographed. The eluent used is cyclohexane containing an increasing proportion of ethyl acetate.

후처리

  1. extractionextracted with diethyl ether
  2. washThe ether phase is washed with sodium thiosulphate solution
  3. customdried
  4. concentrationconcentrated
  5. customchromatographed

출처 및 근거

ORD 기록
ord-f1645386bb714d2d9c8a0c8c7f0e3c48
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06573263B2

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