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Die spontane Spaltung von 3,3-Diäthyl-5-methylpiperidin-2,4-dion(Methyprylon) in die optischen Isomeren. Eine Rötgenstrukturanalyse eines isodimorphen Systems von Mischkristallen

✍ Scribed by Willi E. Oberhänsli


Publisher
John Wiley and Sons
Year
1982
Tongue
German
Weight
522 KB
Volume
65
Category
Article
ISSN
0018-019X

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✦ Synopsis


The Spontaneous Resolution of the 3,3‐Diethyl‐5‐methylpiperidine‐2,4‐dione (Methyprylon) into its Optical Isomers. An X‐Ray Structure Analysis of an Isodimoophous System of Mixed Crystals

Repeated recrystallizations from acetone of a racemic mixture of the title compound successively result in a spontaneous resolution into optical isomers [1]. In this process batches of mixed crystals of increased optical purity are formed [2]. This phenomena was investigated on a molecular basis using X‐ray diffraction methods. The mixed crystals belong to the space group __P__2~1~2~1~2~1~ and their diffraction patterns give no indication of major disorders. There is a linear relationship between the changes in unit cell parameters a and b and the optical rotation of the sample. The structures of the mixed crystals from four fractions belonging to two different crystalline modifications have been determined. The molecular shape is such that most of the atomic positions of the two enantiomers superimpose almost perfectly. Occupation factors determined for the asymmetric C‐ sites agree well with the optical activity of the crystals fraction.


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Spontane Spaltung von 2,4-Dioxo-3,3-diät
✍ K. Vogler; M. Kofler 📂 Article 📅 1956 🏛 John Wiley and Sons 🌐 German ⚖ 512 KB

## Abstract 2, 4‐Dioxo‐3, 3‐diethyl‐5‐methyl‐piperidine is spontaneously re‐ solved into its optical antipodes by about 400 crystallisations from various solvents e.g. methanol, acetone, butanol, water etc. From the melting point diagram and the behaviour in the resolution process it must be conclu