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

HRID 385576
ノート
印刷プレビュー

反応式

HRID 385576 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

反応条件

温度
45 °C

実験手順

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.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-0d418178abfd44ad860a33e3224513dd
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367831B2

反応ノート

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