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Water → HCID 10892558, 화합물

HRID 2299565
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HRID 2299565 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 521998p-Toluenesulfonic acid monohydrateHCID 10924734HCID 10924734, 화합물2회

생성물 1

HCID 10892558HCID 10892558, 화합물수율 187.8%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

The compound (3) (65.47 g, 183 mmol) obtained in above (2) was dissolved in 1,2-dimethoxyethane (1.6 L) 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%.

후처리

  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

출처 및 근거

ORD 기록
ord-e834ff547636411b97b1a8c7f26ad98b
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06495702B2

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