3-Benzyl-1-(4'-methoxybenzyl)-2,5-dioxo-4,4-dimethylimidazolidine → 3-Benzyl-2,5-dioxo-4,4-dimethylimidazolidine

HRID 1978026

반응식

HRID 1978026 반응식
[CH2:1]([N:8]1[C:12]([CH3:14])([CH3:13])[C:11](=[O:15])[N:10](CC2C=CC(OC)=CC=2)[C:9]1=[O:25])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N+]([O-])([O-])=O.[Ce].[NH4+]>C(#N)C.O.C(OCC)(=O)C>[CH2:1]([N:8]1[C:12]([CH3:14])([CH3:13])[C:11](=[O:15])[NH:10][C:9]1=[O:25])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 2

HCID 217000233-Benzyl-1-(4'-methoxybenzyl)-2,5-dioxo-4,4-dimethylimidazolidineHCID 57418452Ammonium cerium-nitrate

생성물 1

HCID 46019883-Benzyl-2,5-dioxo-4,4-dimethylimidazolidine수율 63%

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

반응 조건

온도
25 °C

실험 절차

A solution of 3-benzyl-1-(4′-methoxybenzyl)-2,5-dioxo-4,4-dimethylimidazolidine (3.9 g, 11.54 mmol) in acetonitrile (100 mL) was treated with a solution of ammonium cerium nitrate (31 g, 57.7 mmol) in 65 mL of water, stirred at 25° C. for 15 minutes, then diluted with ethyl acetate and partitioned between ethyl acetate and brine. The organic layer was dried, filtered, and concentrated. Purification by recrystalization with ethyl acetate/hexane provided 1.58 g (7.25 mmol, 63%) of the desired product as white solid.

후처리

  1. custompartitioned between ethyl acetate and brine
  2. customThe organic layer was dried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customPurification
  6. customby recrystalization with ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-fae5a3e119b24dd999adacb62565b9ba
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235786B1

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