p-Toluenesulfonic acid monohydrate → HCID 18615089, 화합물

HRID 565450

반응식

HRID 565450 반응식
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[OH2:15].[C:16]1([CH3:26])C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.C(O)CO>[CH2:16]1[O:15][C:1]([C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=2)([CH3:2])[O:3][CH2:26]1

참가 물질

5

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 600911Ethyl 4-acetylbenzoate

생성물 1

HCID 18615089HCID 18615089, 화합물

시약·촉매·용매 2

HCID 174Ethylene Glycol용매HCID 1140Toluene용매

실험 절차

ethyl 4-acetyl-benzoate (9.61 g, a product of the firm Wako Pure Chemical Ind.) was dissolved in toluene (200 ml) under an argon atmosphere whereto ethylene glycol (20 ml) and p-toluenesulfonic acid hydrate (200 mg) were added, whereupon the mixture was refluxed with heating for 24 hours while dehydrating on a Dean-Stark apparatus. After cooling down to room temerature, the toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly, followed by drying and concentrating to dryness under reduced pressure, whereby the above-identified compound was obtained (12.76 g).

후처리

  1. additionwere added, whereupon the mixture
  2. temperaturewas refluxed
  3. temperaturewith heating for 24 hours
  4. temperatureAfter cooling down to room temerature
  5. washthe toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly
  6. customby drying
  7. concentrationconcentrating to dryness under reduced pressure, whereby the above-identified compound
  8. customwas obtained (12.76 g)

출처 및 근거

ORD 기록
ord-4162c50c57c448d4880a91b9ace26986
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172099B2

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