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Ethylene Glycol → HCID 21999137, 화합물

HRID 1976752
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HRID 1976752 반응식
[CH3:1][CH:2]1[CH:7]([S:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH2:6][CH2:5][CH2:4][C:3]1=[O:17].[CH2:18](O)[CH2:19][OH:20].C(=O)(O)[O-].[Na+]>C1C=CC=CC=1>[CH2:18]1[CH2:19][O:20][C:3]2([CH2:4][CH2:5][CH2:6][CH:7]([S:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)(=[O:10])=[O:9])[CH:2]2[CH3:1])[O:17]1
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참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 516892Sodium BicarbonateHCID 21999124HCID 21999124, 화합물

생성물 1

HCID 21999137HCID 21999137, 화합물수율 95%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution obtained by dissolving 1.4 g of 2-methyl-3-(phenylsulfonyl)-cyclohexan-1-one in 20 ml of benzene, were added 0.41 ml of 1,2-ethanediol and 0.1 g of anhydrous paratoluenesulfonic acid. The resulting mixture was heated under reflux for 4 hours. After the reaction, a 2M aqueous sodium bicarbonate solution was added and the resulting mixture was extracted with ethyl acetate three times. The combined organic layers were washed with saturated saline and dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl ether, whereby 1,1-(ethylenedioxy)-2-methyl-3-(phenylsulfonyl)-cyclohexane was obtained in the form of white crystals. Yield: 95%

후처리

  1. customTo a solution obtained
  2. temperatureThe resulting mixture was heated
  3. temperatureunder reflux for 4 hours
  4. customAfter the reaction
  5. extractionthe resulting mixture was extracted with ethyl acetate three times
  6. washThe combined organic layers were washed with saturated saline
  7. dry with materialdried over magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure
  9. customThe residue was recrystallized from ethyl ether

출처 및 근거

ORD 기록
ord-14d096212c99488faf173d33f022c79b
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06228893B1

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