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Benzoic Acid → 3-Oxobutan-2-yl benzoate

HRID 1290822
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HRID 1290822 반응식
Cl[CH:2]([CH3:6])[C:3](=[O:5])[CH3:4].[C:7]([OH:15])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C>C(#N)C>[C:7]([O:15][CH:2]([CH3:6])[C:3](=[O:5])[CH3:4])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 243Benzoic AcidHCID 8471TriethylamineHCID 200263-Chloro-2-butanone

생성물 1

HCID 2319833-Oxobutan-2-yl benzoate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 3-chlorobutanone (10.6 g), benzoic acid (15.0 g), triethylamine (30 ml) and acetonitrile (100 ml) was heated under reflux for 1 hour 30 minutes. The mixture was cooled and filtered to remove precipitated triethylamine hydrochloride. The acetonitrile was removed from the filtrate under reduced pressure and the residue dissolved in ethyl acetate and washed with water. The organic extracts were dried over magnesium sulphate, filtered over active carbon and the solvent was removed from the filtrate under reduced pressure, to give a yellow oil of 3-benzoyloxybutan-2-one. Yield 16.7 g. The oil was used directly without further purification in the next step.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour 30 minutes
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. customto remove
  6. customprecipitated triethylamine hydrochloride
  7. customThe acetonitrile was removed from the filtrate under reduced pressure
  8. dissolutionthe residue dissolved in ethyl acetate
  9. washwashed with water
  10. dry with materialThe organic extracts were dried over magnesium sulphate
  11. filtrationfiltered over active carbon
  12. customthe solvent was removed from the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-9b21958bae674b96a195899ade3e7919
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753665

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