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2-Amino-4-methylpyridine → 4-Methyl-2-phthalimidopyridine

HRID 726667
ノート
印刷プレビュー

反応式

HRID 726667 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=1.[C:9]1(=O)[O:14][C:12](=[O:13])[C:11]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:10]12.C(OC(=O)C)(=O)C>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([N:8]2[C:12](=[O:13])[C:11]3=[CH:15][CH:16]=[CH:17][CH:18]=[C:10]3[C:9]2=[O:14])[CH:3]=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 3

HCID 15332-Amino-4-methylpyridineHCID 6811Phthalic AnhydrideHCID 7918Acetic Anhydride

生成物 1

HCID 109990494-Methyl-2-phthalimidopyridine収率 42.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a stirring solution of 4-methyl-2-aminopyridine (50 g, 460 mmol) in acetic acid (1 L) was added phthalic anhydride (68 g, 460 mmol) and the reaction was heated to reflux. After 12 h, acetic anhydride (43 mL, 460 mmol) was added and the solution continued to stir at reflux for an additional 48 h. The solvent was then removed in vacuo and the solid residue was suspended in toluene and concentrated in vacuo twice. The solid was then suspended in ethyl acetate with vigorous stirring and filtered. After repeating this ethyl acetate washing procedure the solid was dried overnight in vacuo to give 46.6 g (42%) of a white solid.

後処理

  1. temperaturethe reaction was heated to reflux
  2. temperatureat reflux for an additional 48 h
  3. customThe solvent was then removed in vacuo
  4. concentrationconcentrated in vacuo twice
  5. stirringwith vigorous stirring
  6. filtrationfiltered
  7. customwas dried overnight in vacuo

出典と根拠

ORDレコード
ord-d92e905386224161a9f1d33d433d2443
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05710130

反応ノート

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