Sodium Bicarbonate → 1-(2,4-Dihydroxyphenyl)-3-(4-Hydroxyphenyl)Prop-2-En-1-One
Reaktionsgleichung
[OH:1][C:2]1[CH:21]=[C:20]([O:22]COC)[CH:19]=[CH:18][C:3]=1[C:4](=[O:17])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][C:10]([O:13]COC)=[CH:9][CH:8]=1.Cl.CO.C(=O)([O-])O.[Na+]>O1CCCC1>[OH:1][C:2]1[CH:21]=[C:20]([OH:22])[CH:19]=[CH:18][C:3]=1[C:4](=[O:17])[CH:5]=[CH:6][C:7]1[CH:8]=[CH:9][C:10]([OH:13])=[CH:11][CH:12]=1Komponenten
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
Then, 1.0 g of 2'-hydroxy-4,4'-bis(methoxymethoxy)chalcone was dissolved in 7 ml of tetrahydrofuran, and a 5-15% hydrochloric acid/methanol reagent was added to the solution and the mixture was heated at 50° C. for 30 minutes to effect a reaction. After the reaction, the reaction mixture was neutralized with a saturated aqueous solution of sodium hydrogencarbonate and extracted with 300 ml of ethyl acetate, and the ethyl acetate layer was washed with water (100 ml×3 times), shaken with a saturated aqueous solution of sodium chloride (50 ml×2 times), dried with anhydrous sodium sulfate and filtered. The solvent was removed from the filtrate by distillation, and the obtained residue was subjected to the silica gel column chromatography using a mixed solvent of n-hexane and ethyl acetate to obtain 521 mg (yield=70%) of 2',4,4'-trihydroxychalcone in the form of a yellow grain.
Aufarbeitung
- customa reaction
- customAfter the reaction
- extractionextracted with 300 ml of ethyl acetate
- washthe ethyl acetate layer was washed with water (100 ml×3 times)
- dry with materialdried with anhydrous sodium sulfate
- filtrationfiltered
- customThe solvent was removed from the filtrate by distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-4b729c7856d34a938307bc6913b66552
- Quelldatensatz
- uspto-grants-1993_08
- Patentnummer
- US05234951
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