Hydrogen Bromide → HCID 22033294, Verbindung

HRID 1792314Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1792314
C[O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:22])[C:8]([C:14]3[CH:19]=[CH:18][C:17]([O:20]C)=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1.Br>C(O)(=O)C>[OH:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:22])[C:8]([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1

Komponenten

4

Edukt 2

HCID 260Hydrogen BromideHCID 109799547-Methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one

Produkt 1

HCID 22033294HCID 22033294, VerbindungAusbeute 92,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

To a solution of 7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one (2.27 g, 7.22 mmol) in acetic acid (75 ml) was added 48% aqueous HBr solution (75 mg), which was then heated under reflux for 1 day. The reaction mixture was extracted with diethyl ether. The organic layer was washed with saturated sodium bicarbonate solution and saturated saline solution, dried over anhydrous magnesium sulfate, and concentrated. Then, the residue was subjected to flash chromatography on silica gel (n-hexane:ethyl acetate=7:3 and 1:1) to give the title compound (1.92 g, yield 92%).

Aufarbeitung

  1. temperaturewas then heated
  2. temperatureunder reflux for 1 day
  3. extractionThe reaction mixture was extracted with diethyl ether
  4. washThe organic layer was washed with saturated sodium bicarbonate solution and saturated saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-1fa491b162164f098d0ec14018659b67
Quelldatensatz
uspto-grants-2006_07
Patentnummer
US07074819B2

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