Reaktionsgleichung
[OH-].[K+].[ClH:3].C[O:5][C:6](=[O:23])[CH:7]=[C:8]1[CH2:13][CH2:12][C:11]([N:20]([CH3:22])[CH3:21])([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:10][CH2:9]1.CCOCC.Cl>C(O)C>[ClH:3].[CH3:22][N:20]([CH3:21])[C:11]1([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:12][CH2:13][C:8](=[CH:7][C:6]([OH:23])=[O:5])[CH2:9][CH2:10]1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
1.7 M KOH (70.5 ml, 120 mmol) was added to a solution of (4-dimethylamino-4-phenylcyclohexylidene)acetic acid methyl ester hydrochloride (1.8 g, 5.8 mmol) in ethanol (200 ml) and the mixture was stirred at RT for 16 h. The reaction mixture was concentrated and the residue was taken up in water (40 ml). The aqueous phase was extracted by shaking with ether (2×40 ml), and 5.5 M hydrochloric acid (23.6 ml, 130 mmol) was added. After the aqueous phase had been concentrated, the residue was extracted with ethanol (2×40 ml), the potassium chloride which remained was separated off and the filtrate was concentrated. The hydrochloride of the acid was thereby obtained as a colourless solid in a yield of 98% (1.67 g).
Aufarbeitung
- concentrationThe reaction mixture was concentrated
- extractionThe aqueous phase was extracted
- additionwas added
- concentrationAfter the aqueous phase had been concentrated
- extractionthe residue was extracted with ethanol (2×40 ml)
- customthe potassium chloride which remained was separated off
- concentrationthe filtrate was concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-c1b813893309407887b16d63fe4d1012
- Quelldatensatz
- uspto-grants-2011_09
- Patentnummer
- US08017630B2
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