Sulfuric Acid → HCID 67884339, Verbindung

HRID 257475Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 257475
[N:1]1[CH:6]=[CH:5][C:4]([C:7](O)([CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH3:8])=[CH:3][CH:2]=1.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O>[C:11]1([CH2:10]/[CH:9]=[C:7](/[C:4]2[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=2)\[CH3:8])[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1.[C:11]1([CH2:10][CH2:9][C:7]([C:4]2[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=2)=[CH2:8])[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

Komponenten

6

Edukt 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 19783310HCID 19783310, Verbindung

Produkt 2

HCID 19783363HCID 19783363, VerbindungAusbeute 11,5 %HCID 67884339HCID 67884339, VerbindungAusbeute 33,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To the said alcoholic substance, that is 1.42 g of 2-(4-pyridyl)-4-phenyl-2-butanol, 4 ml of 65% sulfuric acid was added and the mixture was stirred for two hours at 100° C. After cooling, water was added and the mixture was alkalized with sodium carbonate to extract with ethyl acetate. After drying over anhydrous sodium sulfate, the solvent was distilled away under reduced pressure to obtain viscous oily substance. The said oily substance was purified by silica gel column chromatography to obtain 0.44 g of (E)-1-phenyl-3-(4-pyridyl)-2-butene (yield: 33.7%) and 0.15 g of 4-phenyl-2-(4-pyridyl)-1-butene (yield: 11.5%).

Aufarbeitung

  1. additionwas added
  2. temperatureAfter cooling
  3. extractionto extract with ethyl acetate
  4. dry with materialAfter drying over anhydrous sodium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. customto obtain viscous oily substance
  7. customThe said oily substance was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-25d3738c78eb4924a4fa67351b6c44af
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05262420

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