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p-Toluenesulfonic acid → 4-(1,3-Thiazol-2-yl)phenol

HRID 2120270
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HRID 2120270 반응식
COO[CH:4](OOC)[CH2:5]Br.C1(C)C=CC(S(O)(=O)=O)=CC=1.[OH:21][C:22]1[CH:30]=[CH:29][C:25]([C:26]([NH2:28])=[S:27])=[CH:24][CH:23]=1>C(O)C>[S:27]1[CH:5]=[CH:4][N:28]=[C:26]1[C:25]1[CH:29]=[CH:30][C:22]([OH:21])=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 27593444-HydroxythiobenzamideHCID 22352361Bromoacetaldehyde dimethoxyacetal

생성물 1

HCID 2238404-(1,3-Thiazol-2-yl)phenol수율 61.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In a round-bottomed flask, bromoacetaldehyde dimethoxyacetal (123 μl, 1.04 mmol), p-toluenesulfonic acid (199 mg, 1.04 mmol), and 4-hydroxy-thiobenzamide (160 mg, 1.04 mmol) were dissolved in ethanol (10 ml) and the resulting solution was heated to reflux for about twenty-four hours. The reaction mixture was then concentrated to an oil which was redissolved in ethyl acetate, and extracted with saturated aqueous sodium carbonate. The combined organic extracts were then washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo to an oil. The crude product was purified by column chromatography (hexanes to 10% ethyl acetate/hexanes) to furnish the title compound as a white solid (113 mg, 61% yield). LRMS ([M+H+])=177.8.

후처리

  1. temperaturethe resulting solution was heated
  2. temperatureto reflux for about twenty-four hours
  3. concentrationThe reaction mixture was then concentrated to an oil which
  4. dissolutionwas redissolved in ethyl acetate
  5. extractionextracted with saturated aqueous sodium carbonate
  6. washThe combined organic extracts were then washed with brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo to an oil
  10. customThe crude product was purified by column chromatography (hexanes to 10% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-1388a77f06b2477086dc604dfaae3653
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06689888B2

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