Water → HCID 18670149、化合物

HRID 1059388ノート

反応式

HRID 1059388 の反応式
[H-].[Na+].[NH:3]1[CH:7]=[CH:6][N:5]=[C:4]1[CH2:8][NH:9][C:10](=[O:12])[CH3:11].[CH3:13][Si:14]([CH3:21])([CH3:20])[CH2:15][CH2:16][O:17][CH2:18]Cl.O>CN(C)C=O.C(OCC)(=O)C>[CH3:13][Si:14]([CH3:21])([CH3:20])[CH2:15][CH2:16][O:17][CH2:18][N:3]1[CH:7]=[CH:6][N:5]=[C:4]1[CH2:8][NH:9][C:10](=[O:12])[CH3:11]

参加物

7

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 27242712-Chloromethyl 2-(trimethylsilyl)ethyl etherHCID 18670192N-[(1H-imidazol-2-yl)methyl]acetamide

生成物 1

HCID 18670149HCID 18670149、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

Under ice-cooling, 0.08 g of sodium hydride (60% oily) was added to a solution of 0.31 g of N-(imidazol-2-ylmethyl)acetamide in N,N-dimethylformamide (10 ml). After stirring for 15 minutes, a solution of 0.35 ml of 2-(trimethylsilyl)ethoxymethyl chloride in N,N-dimethylformamide (1 ml) was dropped thereinto and the resulting mixture was stirred at room temperature for additional 16 hours. Then the reaction mixture was distributed into water and ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. After concentrating under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 0.16 g of the title compound as a colorless oily substance.

後処理

  1. temperatureUnder ice-cooling
  2. stirringthe resulting mixture was stirred at room temperature for additional 16 hours
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationAfter concentrating under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)

出典と根拠

ORDレコード
ord-c14974c2712e4042a06800136c02682d
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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