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Assymetryc catalisys in organic chemistry by Noyori R

By Noyori R

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Reste von Lösemitteln, die zum Entfetten verwendet werden, müssen durch Abblasen mit ölfreier Luft entfernt werden. Für Sauerstoff dürfen nur Manometer verwendet werden, die blau gekennzeichnet sind und die Aufschrift „Sauerstoff! " tragen. Für Präparationen im Halbmikromaßstab haben sich kleine Druckgasflaschen mit Gasmengen zwischen 200-450 g, die bequem in jedem Abzug neben der entsprechenden Apparatur installierbar sind, bewährt. Eine Übersicht erhältlicher Gase befindet sich in vielen Feinchemikalien-Katalogen.

Die Umkristallisation wird bis zur Konstanz der Schmelztemperatur wiederholt. Sehr kleine Mengen an Festsubstanzen werden im Craig-Röhrchen mit Tefloneinsatz (Abb. 35a für 2 bzw. 3 ml Inhalt) vom Lösungsmittel befreit. ). Durch das Loch im Tefloneinsatz wird ein Draht gezogen, der beiderseits aus dem Zentrifugenglas hängt. Man zentrifugiert vorsichtig, so daß sich das Teflon nicht verbiegt. Tefloneinsätze, die sich am herausragenden Ende nicht verjüngen, sind grundsätzlich vorzuziehen. Das beim Übergang vom breiten zum schmalen Teil etwas angeschliffene Röhrchen gestattet nur dem Lösungsmittel den Durchtritt.

Bei höher siedenden Substanzen stellt man daher mittels eines Manostaten ein geeignetes Vakuum ein, das grundsätzlich erst dann angelegt wird, wenn sich der Rührer bewegt. Bei den kleinen Destillatmengen ist es wichtig, daß man zur Innentemperaturmessung ein empfindliches Thermometer verwendet, andernfalls wird eine zu niedrige Temperatur angezeigt. Als Wärmeüberträger können kleine Ölbäder oder mit entsprechenden Aussparungen versehene Metallblöcke, die auf einem heizbaren Magnetrührwerk sitzen, dienen.

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