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Water → HCID 10892558、化合物

HRID 430005
ノート
印刷プレビュー

反応式

HRID 430005 の反応式
[C:1]1([S:7]([O:10][C:11]2[CH:16]=[CH:15][C:14]([S:17][CH2:18][C:19]#[CH:20])=[CH:13][CH:12]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.O.C1(C)C=CC(S(O)(=O)=[O:30])=CC=1>COCCOC>[C:1]1([S:7]([O:10][C:11]2[CH:12]=[CH:13][C:14]3[S:17][CH:18]=[C:19]([CH2:20][OH:30])[C:15]=3[CH:16]=2)(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物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 962WaterHCID 521998p-Toluenesulfonic acid monohydrateHCID 10924734HCID 10924734、化合物2 回

生成物 1

HCID 10892558HCID 10892558、化合物収率 187.8%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

The compound (3) (65.47 g, 183 mmol) obtained in above (2) was dissolved in 1,2-dimethoxyethane (1.6L) and the solution was refluxed for 4 hours. To the solution were added water (64 ml) and p-toluenesulfonic acid monohydrate (19.2 g, 100 mmol) and refluxing was continued for 2 hours. The reaction mixture was concentrated under reduced pressure. After water (200 ml) was added to the resulting oil, the mixture was extracted with ethyl acetate (300 ml). The organic layer was washed with aqueous sodium hydrogen carbonate and water, dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure to provide 60.18 g of the title compound (4) as oil. Crude yield: 103%.

後処理

  1. temperaturethe solution was refluxed for 4 hours
  2. temperaturerefluxing
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionAfter water (200 ml) was added to the resulting oil
  5. extractionthe mixture was extracted with ethyl acetate (300 ml)
  6. washThe organic layer was washed with aqueous sodium hydrogen carbonate and water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-d27b620dbe844f5e9ac5a9a1249e15b8
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06320060B1

反応ノート

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