Ethanol → HCID 14650456, Verbindung

HRID 1200195Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1200195
Br[C:2]1([C:8]2[O:9][C:10]3[C:18]([CH2:19][C:20]#N)=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:14])[CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.S(=O)(=O)(O)[OH:23].[CH2:27]([OH:29])[CH3:28]>>[C:2]1([C:8]2[O:9][C:10]3[C:18]([CH2:19][C:20]([O:29][CH2:27][CH3:28])=[O:23])=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:14])[CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=1

Komponenten

4

Edukt 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 146504442-(1-Bromocyclohexyl)-8-cyanomethyl-4-oxo-4H-[1]-benzopyran

Produkt 1

HCID 14650456HCID 14650456, VerbindungAusbeute 56 %

Versuchsvorschrift

2-(1-Bromocyclohexyl)-8-cyanomethyl-4-oxo-4H-[1]-benzopyran (5.0 g) and 50% sulfuric acid (4 ml) were added to ethanol (400 ml) and the mixture was refluxed for 8 hours. Then, ethanol (about 300 ml) was distilled off under reduced pressure and the residue was added to water. The mixture was extracted with ethyl acetate and the extract was washed with water, dried (MgSO4) and concentrated. The residue was recrystallized from ethyl acetate to obtain the title compound, yield 56%.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 8 hours
  2. distillationThen, ethanol (about 300 ml) was distilled off under reduced pressure
  3. additionthe residue was added to water
  4. extractionThe mixture was extracted with ethyl acetate
  5. washthe extract was washed with water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customThe residue was recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-91715fe907ea4772961b884df4ebe04a
Quelldatensatz
uspto-grants-1990_02
Patentnummer
US04904690

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