Hydrochloric Acid → 5-(2-Hydroxy-3,4-dimethoxyphenyl)isoindolin-1-one
Reaktionsgleichung
[CH3:1][O:2][C:3]1[C:4]([O:21]COC)=[C:5]([C:11]2[CH:12]=[C:13]3[C:17](=[CH:18][CH:19]=2)[C:16](=[O:20])[NH:15][CH2:14]3)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].Cl>CO>[OH:21][C:4]1[C:3]([O:2][CH3:1])=[C:8]([O:9][CH3:10])[CH:7]=[CH:6][C:5]=1[C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[C:16](=[O:20])[NH:15][CH2:14]2Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
To a stirring solution of 5-(3,4-dimethoxy-2-(methoxymethoxy)phenyl)isoindolin-1-one (600 g, 1.81 mmol) in methanol (20 mL) at 0° C., was added concentrated hydrochloride acid (1 mL) and the resultant reaction mixture was stirred at 50° C. for 15 min. The reaction mixture was concentrated under reduced pressure and basified with aq sodium bicarbonate solution extracted with ethyl acetate (3×). The combined ethyl acetate layer was washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. Purification of the resulting residue by washings with ether afforded the title compound as a solid.
Aufarbeitung
- customthe resultant reaction mixture
- concentrationThe reaction mixture was concentrated under reduced pressure and basified with aq sodium bicarbonate solution
- extractionextracted with ethyl acetate (3×)
- washThe combined ethyl acetate layer was washed with brine
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated under reduced pressure
- customPurification of the resulting residue
- washby washings with ether
Quellen und Nachweise
- ORD-Eintrag
- ord-2f9a5bdac5904cf38b07246842438006
- Quelldatensatz
- uspto-grants-2015_06
- Patentnummer
- US09051290B2
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