Reaktionsgleichung
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][O:7][C:8]2=[O:9])=[CH:4][CH:3]=1.[C:12]1([O-:18])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Na+].Cl>O>[O:18]([CH2:6][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:11][C:10]=1[C:8]([OH:7])=[O:9])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
Stir a mixture of 1.0 gm of 6-methylphthalide and 0.64 gm of sodium phenolate at a temperature of 200°-210° C. for 1 hour. Cool and dissolve the reaction mixture in water. Acidify with 5% hydrochloric acid and extract with ether. Evaporate to dryness and chromatograph the residue over silica gel eluting with chloroform/methanol (50:1). Evaporate the eluate to dryness and crystallize the residue from ethyl acetate/benzene to obtain the title product.
Aufarbeitung
- temperatureCool
- extractionextract with ether
- customEvaporate to dryness and chromatograph the residue over silica gel eluting with chloroform/methanol (50:1)
- customEvaporate the eluate to dryness
- customcrystallize the residue from ethyl acetate/benzene
Quellen und Nachweise
- ORD-Eintrag
- ord-b246f9bd4a88459493a5078507417c1d
- Quelldatensatz
- uspto-grants-1981_08
- Patentnummer
- US04282365
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