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7-Methyl-1,8-naphthyridin-2-ol → 7-Methyl-3,4-dihydro-1,8-naphthyridin-2(1H)-one

HRID 385576
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HRID 385576 반응식
[CH3:1][C:2]1[N:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1>C(O)C.[C].[Pd]>[CH3:1][C:2]1[N:11]=[C:10]2[C:5]([CH2:6][CH2:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 53736757-Methyl-1,8-naphthyridin-2-ol

생성물 1

HCID 578152267-Methyl-3,4-dihydro-1,8-naphthyridin-2(1H)-one수율 45.4%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

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온도
45 °C

실험 절차

A solution of 2.0 g of 7-methyl-1,8-naphthyridin-2(1H)-one in 150 mL of ethanol, 1.0 g of 5% palladium-carbon was added, and the mixture was stirred at 40 to 50° C. for 17 hours under a hydrogen atmosphere. The reaction mixture was cooled to room temperature, the insoluble substance was filtered off, and the filtration residue was washed with methanol. The solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography using an eluent of hexane:ethyl acetate=1:1 to obtain 0.92 g of 7-methyl-3,4-dihydro-1,8-naphthyridin-2(1H)-one as a white solid.

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후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationthe insoluble substance was filtered off
  3. washthe filtration residue was washed with methanol
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe resultant residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-0d418178abfd44ad860a33e3224513dd
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367831B2

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