Dimethylformamide → N-[(1H-imidazol-2-yl)methyl]acetamide

HRID 1059387ノート

反応式

HRID 1059387 の反応式
Cl.Cl.[NH2:3][CH2:4][C:5]1[NH:6][CH:7]=[CH:8][N:9]=1.CN(C)C=O.[H-].[Na+].[C:17](OC(=O)C)(=[O:19])[CH3:18]>N1C=CC=CC=1>[NH:6]1[CH:7]=[CH:8][N:9]=[C:5]1[CH2:4][NH:3][C:17](=[O:19])[CH3:18]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 24758Sodium hydrideHCID 124178631H-imidazol-2-ylmethanamine dihydrochloride

生成物 1

HCID 18670192N-[(1H-imidazol-2-yl)methyl]acetamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

0.34 g of 2-aminomethylimidazole dihydrochloride was added to 20 ml of N,N-dimethylformamide in a nitrogen atmosphere. Under ice-cooling, 0.40 g of sodium hydride (60% oily) was added thereto and the resulting mixture was subjected to ultrasonication for 30 minutes. To the reaction mixture were added 20 ml of pyridine and 10 ml of acetic anhydride and the obtained mixture was stirred at room temperature for 2 days. After concentrating under reduced pressure, the residue was distributed into water and ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulfate. The extract was concentrated under reduced pressure to thereby give 0.24 g of the title compound as a pale brown solid.

後処理

  1. temperatureUnder ice-cooling
  2. customthe resulting mixture was subjected to ultrasonication for 30 minutes
  3. concentrationAfter concentrating under reduced pressure
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationThe extract was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-4d6a00c696fe4de29020fd3a793d9c96
出典データセット
uspto-grants-2003_02
特許番号
US06518423B1

反応ノート

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