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Methyl iodide → HCID 67281758, 화합물

HRID 913037
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HRID 913037 반응식
CI.[CH2:3]([O:10][C:11]1[C:16](=[O:17])[C:15]([CH2:18][C:19]([F:22])([F:21])[F:20])=[CH:14][NH:13][C:12]=1[CH3:23])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[C:24](=O)([O-])[O-].[K+].[K+]>C(#N)C.ClCCl>[CH2:3]([O:10][C:11]1[C:16](=[O:17])[C:15]([CH2:18][C:19]([F:22])([F:21])[F:20])=[CH:14][N:13]([CH3:24])[C:12]=1[CH3:23])[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 67282712HCID 67282712, 화합물

생성물 1

HCID 67281758HCID 67281758, 화합물수율 95%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

Methyl iodide (11 mL, 176 mmol) was added to a suspension of 3-benzyloxy-2-methyl-5-(2,2,2-trifluoro-ethyl)-1H-pyridin-4-one (1.18 g, 4.0 mmol) and potassium carbonate (1.06 g, 7.7 mmol) in acetonitrile (25 mL). The resulting mixture was heated to reflux, and the reaction was completed within 40 min. The mixture was cooled to RT, and the solid particulates was filtered off. The filtrate was concentrated in vacuo to give a solid. The solid was taken up in dichloromethane, and the organic layer was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to afford 3-benzyloxy-1,2-dimethyl-5-(2,2,2-trifluoro-ethyl)-1H-pyridin-4-one as a colorless oil (1.3 g, 95% yield, HPLC Method 1 (Example 24), RT=15.9 min, HPLC purity (peak percent area): 98% at λ=280 nm).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux
  3. filtrationthe solid particulates was filtered off
  4. concentrationThe filtrate was concentrated in vacuo
  5. customto give a solid
  6. washthe organic layer was washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3531663430e6481b84c1b2bf55e42866
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08026261B2

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