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Hydrochloric Acid → 2-Methyl-1,8-naphthyridin-3-ol

HRID 228900
ノート
印刷プレビュー

反応式

HRID 228900 の反応式
[NH2:1][C:2]1[C:7]([CH:8]=O)=[CH:6][CH:5]=[CH:4][N:3]=1.Cl[CH2:11][C:12](=O)[CH3:13].Cl.[OH-:16].[Na+]>>[CH3:13][C:12]1[C:11]([OH:16])=[CH:8][C:7]2[C:2](=[N:3][CH:4]=[CH:5][CH:6]=2)[N:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 6571ChloroacetoneHCID 14798Sodium HydroxideHCID 7376333-Pyridinecarboxaldehyde, 2-amino-

生成物 1

HCID 230782942-Methyl-1,8-naphthyridin-3-ol収率 40%

実験手順

2-Amino-pyridine-3-carbaldehyde (2.0 g) and chloroacetone (1.5 g) were suspended in a 5 N aqueous sodium hydroxide solution (10 ml) and was allowed to stand in a hermetically sealed state for 3 days. The reaction solution was neutralized with 10% hydrochloric acid, and the precipitated crystal was then collected by filtration. Isopropanol was added to the crystal, and the mixture was heated under reflux. The reaction solution was cooled to room temperature, and the solvent was then removed by distillation. Hexane was added to the residue, and the precipitated crystal was collected by filtration and was washed with hexane to give 2-methyl-[1,8]naphthyridin-3-ol (1.05 g, yield 40%).

後処理

  1. filtrationthe precipitated crystal was then collected by filtration
  2. additionIsopropanol was added to the crystal
  3. temperaturethe mixture was heated
  4. temperatureunder reflux
  5. customthe solvent was then removed by distillation
  6. additionHexane was added to the residue
  7. filtrationthe precipitated crystal was collected by filtration
  8. washwas washed with hexane

出典と根拠

ORDレコード
ord-b029443dce724409aa24acac54e5274d
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07560558B2

反応ノート

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