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

HRID 726667
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반응식

HRID 726667 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 109990494-Methyl-2-phthalimidopyridine수율 42.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d92e905386224161a9f1d33d433d2443
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05710130

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