Über Pterinchemie 76. Mitteilung [1] Eine einfache Synthese von Leucovorin

A Convenient Synthesis of Leucovorin The synthesis of leucovorin, a 5-formyl-(6R or S)-5,6,7,8-tetrahydropteroyl-L -glutamic acid (II) is described. The L -folic acid was first reduced to (6R, S)-tetrahy-dro-L -folic acid (I); formylation with methyl-formate in DMSO gave directly leucovorin (as a diastereomeric mixture) in good yields. To demonstrate, that the formylation occurred regiospecifically at N (5) and not at N (10), N (10)-nitroso-(6 R, S)-tetrahydro-L -folic acid was formylated under the same conditions. Reductive elimination of the N (10)-nitrosogroup gave the identical leucovorin as in the previous case. The synthetic leucovorin was biologically as active as the natural product with Streptococcus faecalis ATCC 8043 and Pediococcus cerevisiae ATCC 8081.     

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Cyano-modified pre-coated plates — a medium polar modification for high performance thin-layer chromatography

Summary The introduction of a cyano-modified, pre-coated layer substantially widens the selectivity of stationary phases in thin-layer chromatography. This is a moderately polar sorbent based on silica gel 60, which can be used both in adsorption chromatography and in reversed-phase chromatography. This new pre-coated layer is particularly suitable for separation of steroids, alkaloids and derivatized amino acids. The possibility of separating habitforming drugs and preservatives in the presence of ionpair reagents is also discussed.     

5,6,7,8-Tetrahydro-4H-1,2,5-oxadiazocin-6-one durch Ringerweiterung nach Addition eines 3-Isoxazolidinons mit 3-Amino-2H-azirinen

5,6,7,8-Tetrahydro-4H-1,2,5-oxadiazocin-6-ones, Ring Enlargement Products from a 3-Isoxazolidinone and 3-Amino-2H-azirines 3-Dimethylamino-2H-azirines 1 and 4,4-dimethyl-3-isoxazolidinone ( 7 ) undergo already at room temperature a ring enlargement reaction to yield 5,6,7,8-tetrahydro-4H-1,2,5-oxadiazocines of type 8 . The structure of 8a has been confirmed by X-ray crystallography. The conformation of the eight-membered ring with a trans-amide group is of particular interest (Fig. 1 and 2).     

Acetamidiniumhexafluorometallate von Aluminium,Gallium, Indium,Vanadium, Chrom,Mangan, Eisen und Cobalt

Acetamidiniumhexafluorometallates of Aluminium, Gallium, Indium, Vanadium, Chromium, Manganese, Iron and Cobalt The title compounds were crystallized from F-containing aqueous solutions of their hexafluoro-metallate acids by adding acetamidine. Their unit cells were determined and the thermal decomposition was investigated thermoanalytically. The crystal structure of [CH₃C(NH₂)₂]₃AlF₆ was determined: Space group P4₁2₁2/P4₃2₁2, a = 8,987(1), c = 17,894(3) Å, R = 0,054. The unit cell parameters: .     

Chemische,thermoanalytische und röntgenorgraphische Untersuchungen zur Bildung des β-Ca2[P2O7] aus dem Ca2[P4O12] · 4 H2O

Chemical, Thermoanalytical, and X-ray Investigations to the Formation of the β-Ca₂[P₂O₇] from the Ca₂[P₄O₁₂] · 4 H₂O The formation of β-Ca₂[P₂O₇] from Ca₂[P₄O₁₂] · 4 H₂O (modification I) proceeds crystallographically oriented in several steps: In one of these steps an X-ray amorphous phase is formed and simultaneously cyclotetraphosphate reorganizes to polyphosphate. The dehydration proceeds in 2 steps: At 120°C 3 molecules and at 220°C 1 molecule are lost, respectively. The formation of diphosphate from polyphosphate, which is connected with the loss of P₂O₅, takes place at 850°C according to high temperature Guinier.