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

HRID 1597412
ノート
印刷プレビュー

反応式

HRID 1597412 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6a44f87154ca4a7f97e09c94a115e08e
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06294573B1

反応ノート

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