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

HRID 1728337

반응식

HRID 1728337 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 190029815-Benzyl-4-isopropyl-2-methylimidazole수율 0.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-a74d0aafbbe14ecf9e4b0490286984e7
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05326780

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