Diethyl Ether → HCID 67164894, Verbindung
Reaktionsgleichung
[CH2:1]([N:4]([CH2:23][CH2:24][CH3:25])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:19](OC)=[O:20])[CH:15]=2)[CH2:10]1)[CH2:2][CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].C(OCC)C>O1CCCC1>[CH2:23]([N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([CH2:19][OH:20])[CH:15]=2)[CH2:10]1)[CH2:24][CH3:25]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- -78 °C
Versuchsvorschrift
To a solution of the compound 20 (3.02 g) in tetrahydrofuran (25 mL), lithium aluminum hydride (330 mg) was, added at −78° C. The reaction mixture was stirred at −78° C. for 30 minutes. To the reaction mixture, sodium sulfate decahydrate (2.8 g) and diethylether (100 mL) were added and the temperature of the reaction mixture was raised to room temperature. The reaction mixture was filtered through Celite (trade name) and then concentrated. The residue was purified by silica gel column chromatography (ethyl acetate:methanol:triethylamine=10:1:0→10:1:0.5) to obtain the title compound (2.28 g) having the following physical properties.
Aufarbeitung
- additionadded at −78° C
- temperaturethe temperature of the reaction mixture was raised to room temperature
- filtrationThe reaction mixture was filtered through Celite (trade name)
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (ethyl acetate:methanol:triethylamine=10:1:0→10:1:0.5)
Quellen und Nachweise
- ORD-Eintrag
- ord-ca6219708db847e196d191f4740894cb
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08822459B2
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