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Potassium Carbonate → 3-(3,4,4-Trimethyl-2,5-dioxoimidazolidin-1-yl)-2-methoxymethyloxy-prop-1-ene

HRID 1597412
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HRID 1597412 반응식
[CH3:1][N:2]1[C:8]([CH3:10])([CH3:9])[C:6](=[O:7])[NH:5][C:3]1=[O:4].C(=O)([O-])[O-].[K+].[K+].[CH3:17][O:18][CH2:19][O:20][C:21](=[CH2:24])[CH2:22]Cl>CN(C=O)C>[CH3:1][N:2]1[C:8]([CH3:10])([CH3:9])[C:6](=[O:7])[N:5]([CH2:24][C:21]([O:20][CH2:19][O:18][CH3:17])=[CH2:22])[C:3]1=[O:4]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 812951,5,5-Trimethylimidazolidine-2,4-dioneHCID 106782943-Chloro-2-(methoxymethoxy)prop-1-ene

생성물 1

HCID 217002333-(3,4,4-Trimethyl-2,5-dioxoimidazolidin-1-yl)-2-methoxymethyloxy-prop-1-ene수율 89%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

A mixture of 1,5,5 trimethylhydantoin (7.0 g, 49.2 mmol), powdered potassium carbonate (8.16 g, 59 mmol) and 2-methoxymethyloxy-allyl chloride (7.65 g, 56 mmol) in dry DMF (100 mL) was heated to 100° C. with stirring for 1.5 h. The reaction mixture was cooled, fliltered and the filtrate was concentrated, then partitioned between ethyl acetate and water. The organic extract was washed twice with water, brine, dried and concentrated, then purified via silica gel chromatography eluting with 50% ethyl acetate: hexane to give 10.58 g (89%) of the title compound.

후처리

  1. temperatureThe reaction mixture was cooled
  2. concentrationthe filtrate was concentrated
  3. custompartitioned between ethyl acetate and water
  4. extractionThe organic extract
  5. washwas washed twice with water, brine
  6. customdried
  7. concentrationconcentrated
  8. custompurified via silica gel chromatography
  9. washeluting with 50% ethyl acetate

출처 및 근거

ORD 기록
ord-6a44f87154ca4a7f97e09c94a115e08e
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06294573B1

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