Reaktionsgleichung
[CH3:1][C:2]1[C:7]([CH2:8][C:9]#N)=[CH:6][CH:5]=[CH:4][N:3]=1.S(=O)(=O)(O)O.C(=O)(O)[O-:17].[Na+].[CH2:21]([OH:23])[CH3:22]>>[CH2:21]([O:23][C:9](=[O:17])[CH2:8][C:7]1[C:2]([CH3:1])=[N:3][CH:4]=[CH:5][CH:6]=1)[CH3:22]Komponenten
5
Versuchsvorschrift
790 mg (5.98 mmol) of the compound from Example 38A are initially introduced into 10 ml ethanol, 4 ml concentrated sulfuric acid are added slowly and the mixture is heated under reflux for 6 h. After cooling, the mixture is neutralized with 6.00 g sodium bicarbonate and saturated sodium bicarbonate solution. The aqueous phase is extracted several times with ethyl acetate and the combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue is reacted without further purification.
Aufarbeitung
- additionare added slowly
- temperaturethe mixture is heated
- temperatureunder reflux for 6 h
- temperatureAfter cooling
- extractionThe aqueous phase is extracted several times with ethyl acetate
- dry with materialthe combined organic phases are dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe residue is reacted without further purification
Quellen und Nachweise
- ORD-Eintrag
- ord-26c686c181134a499eb02e8399b224bf
- Quelldatensatz
- uspto-grants-2015_07
- Patentnummer
- US09085572B2
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