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Methanol → HCID 90021077, 화합물

HRID 1487817
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HRID 1487817 반응식
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([C:12](=[O:15])[CH2:13][CH3:14])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:21]O>>[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([C:12](=[O:15])[CH2:13][CH3:14])=[CH:7][C:3]=1[C:4]([O:6][CH3:21])=[O:5]
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참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 900211532,4-Dimethyl-5-propionylbenzoic acid2회

생성물 1

HCID 90021077HCID 90021077, 화합물수율 70%

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온도
70 °C

실험 절차

To a 100-mL round-bottom flask, was carefully added 2,4-dimethyl-5-propionylbenzoic acid (compound 1.4, 1.2 g, 5.8 mmol), sulfuric acid (1.0 mL, 19 mmol) and methanol (30 mL). The resulting solution was stirred at 70° C. for 5 h, then concentrated under reduced pressure. The residue was carefully diluted with H2O (50 mL) and extracted ethyl acetate (100 mL). The organic layer was washed with H2O (2×100 mL) and brine (100 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography with ethyl acetate/petroleum ether (1:100) as the eluent to yield the title compound as a light yellow solid (0.90 g, 70%).

후처리

  1. customTo a 100-mL round-bottom flask, was carefully added
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue was carefully diluted with H2O (50 mL)
  4. extractionextracted ethyl acetate (100 mL)
  5. washThe organic layer was washed with H2O (2×100 mL) and brine (100 mL)
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography with ethyl acetate/petroleum ether (1:100) as the eluent

출처 및 근거

ORD 기록
ord-c6286a8bfd534bdfa8c9d774cf33948c
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428502B2

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