Water → HCID 54136706, Verbindung
Reaktionsgleichung
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14](OC)=[O:15])=[C:12]([CH3:18])[N:11]=[C:10]([CH:19]([CH3:21])[CH3:20])[C:9]=2[C:22](OCC)=[O:23])=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[K+]>O1CCCC1>[OH:23][CH2:22][C:9]1[C:10]([CH:19]([CH3:21])[CH3:20])=[N:11][C:12]([CH3:18])=[C:13]([CH2:14][OH:15])[C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
20.7 g (57.7 mmol) of the compound from Example 26 dissolved in 50 ml of absolute tetrahydrofuran are slowly added dropwise under nitrogen to a suspension of 6 g (158 mmol) of lithium aluminum hydride in 200 ml of absolute tetrahydrofuran at 60° C. The mixture is heated to reflux for 1 h, cooled to 0° C. and 18 ml of water are cautiously added. 6 ml of 10% strength potassium hydroxide solution are added to the mixture, it is filtered off from the precipitate with suction and the residue is boiled twice using 250 ml of ether each time. The combined mother liquors are dried over magnesium sulphate and concentrated in vacuo, The residue is stirred with petroleum ether, filtered off with suction and dried in a desiccator.
Aufarbeitung
- temperatureThe mixture is heated
- temperatureto reflux for 1 h
- filtrationis filtered off from the precipitate with suction
- dry with materialThe combined mother liquors are dried over magnesium sulphate
- concentrationconcentrated in vacuo
- filtrationfiltered off with suction
- customdried in a desiccator
Quellen und Nachweise
- ORD-Eintrag
- ord-2609530195684d0abe5f91e31b0f6633
- Quelldatensatz
- uspto-grants-1996_03
- Patentnummer
- US05502057
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