Ammonium Acetate → 5-Benzyl-4-isopropyl-2-methylimidazole

HRID 2259240ノート

反応式

HRID 2259240 の反応式
[C:1]([NH:4][CH:5]([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6](=O)[CH:7]([CH3:9])[CH3:8])(=O)[CH3:2].C([O-])(=O)C.[NH4+:22]>C(O)(=O)C>[CH2:11]([C:5]1[NH:4][C:1]([CH3:2])=[N:22][C:6]=1[CH:7]([CH3:9])[CH3:8])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 190029664-Acetylamino-2-methyl-5-phenyl-3-pentanone

生成物 1

HCID 190029815-Benzyl-4-isopropyl-2-methylimidazole収率 0.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 1.00 g of 4-acetylamino-2-methyl-5-phenyl-3-pentanone (4.29 mmol) in 20 ml of acetic acid is added 5.00 g of ammonium acetate (64.9 mmol), and the resultant mixture is heated under reflux. One hour later, the reaction mixture is concentrated in vacuo, neutralized with aqueous sodium bicarbonate and extracted with ethyl acetate. The extract is washed with saturated brine, dried over sodium sulfate, filtered and the filtrate is concentrated. The crude product is recrystallized from ether/n-hexane to give 0.90 mg of the objective 5-benzyl-4-isopropyl-2-methylimidazole 6. Yield, 97.5%.

後処理

  1. temperatureunder reflux
  2. concentrationOne hour later, the reaction mixture is concentrated in vacuo
  3. extractionextracted with ethyl acetate
  4. washThe extract is washed with saturated brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate is concentrated
  8. customThe crude product is recrystallized from ether/n-hexane

出典と根拠

ORDレコード
ord-35755198f5c64b0c9e6d82f067a944ca
出典データセット
uspto-grants-1995_12
特許番号
US05472965

反応ノート

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