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2,3-Diaminopyridine → 8-Amino-3-acetyl-2-methylimidazo[1,2-a]pyridine

HRID 1006694
ノート
印刷プレビュー

反応式

HRID 1006694 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.Cl[CH2:10][C:11]([CH2:13][C:14](=O)[CH3:15])=[O:12]>C(O)C>[NH2:8][C:7]1[C:2]2[N:3]([C:13]([C:11](=[O:12])[CH3:10])=[C:14]([CH3:15])[N:1]=2)[CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 99562,3-DiaminopyridineHCID 144968561-Chloro-2,4-pentanedione

生成物 1

HCID 226726498-Amino-3-acetyl-2-methylimidazo[1,2-a]pyridine収率 15.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2,3-diaminopyridine (7 g, 64.1 mmol), 3-chloroacetylacetone (8.6 g, 64.1 mmol) in ethyl alcohol (80 ml) was refluxed for 9 hours. The solvent was removed under reduced pressure and the residue dissolved in methylene chloride. A sodium bicarbonate solution was added and the organic layer was separated. The aqueous layer was extracted twice with methylene chloride. The combined organic layer was dried and evaporated under reduced pressure. Chromatography of the residue on silica gel (methylene chloride:methanol, 100:5) gave a product which after recrystallisation from ethyl acetate gave 1.9 g (15%) of the title compound.

後処理

  1. temperaturewas refluxed for 9 hours
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue dissolved in methylene chloride
  4. additionA sodium bicarbonate solution was added
  5. customthe organic layer was separated
  6. extractionThe aqueous layer was extracted twice with methylene chloride
  7. customThe combined organic layer was dried
  8. customevaporated under reduced pressure
  9. customChromatography of the residue on silica gel (methylene chloride:methanol, 100:5) gave a product which
  10. customafter recrystallisation from ethyl acetate

出典と根拠

ORDレコード
ord-38a461c60e1d4357bd3b2c6fa6275990
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06790960B2

反応ノート

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