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Methyl iodide → 3-Bromo-5-ethyl-6-methoxy-2-methylpyridine

HRID 249736
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HRID 249736 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][CH3:11])[C:5](=[O:9])[NH:6][C:7]=1[CH3:8].[CH3:12]I>C(Cl)(Cl)Cl.C(=O)([O-])[O-].[Ag+2]>[Br:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([O:9][CH3:12])=[C:4]([CH2:10][CH3:11])[CH:3]=1
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참가 물질

5

반응물 2

HCID 6328Methyl iodideHCID 207792745-bromo-3-ethyl-6-methyl-1H-pyridin-2-one

생성물 1

HCID 116586693-Bromo-5-ethyl-6-methoxy-2-methylpyridine수율 6,287.1%

시약·촉매·용매 2

HCID 178418647HCID 178418647, 화합물촉매HCID 6212Chloroform용매

실험 절차

5-Bromo-3-ethyl-6-methyl-1H-pyridin-2-one (25 g, 115.7 mmol) was dissolved in 200 ml of chloroform to form an orange solution. Silver carbonate (31.9 g, 115.7 mmol) was added and the mixture was vigorously stirred. Methyl iodide (10.8 ml, 1.5 mmol) was added to this suspension, which was then stirred in the dark at RT under nitrogen. After 3 days, the mixture was filtered and the solution was concentrated in a rotary evaporator. The residue was chromatographed on silica gel with n-heptane as mobile phase and afforded a colorless oil (21.7 g, 82%).

후처리

  1. customto form an orange solution
  2. stirringwas then stirred in the dark at RT under nitrogen
  3. filtrationthe mixture was filtered
  4. concentrationthe solution was concentrated in a rotary evaporator
  5. customThe residue was chromatographed on silica gel with n-heptane as mobile phase

출처 및 근거

ORD 기록
ord-b6c79297801249f9ad8abeff96178557
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863280B2

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