Recherches sur le cyanure de lithium

Abstract

Cette étude a conduit aux conclusions suivantes: Par action due cyanogène sur le lithium, en présence de fer, on parvient à des mélanges de cyanure et de cyanamide accompagnés de paracyanogène. L'action de l'acide cyanhydrique gezeux sur la lithine, en absence de fer, conduit à des mélanges contenant des quantités de paracyanogène.

Lithium dicyanoargentate(I) acetonitrile disolvate

“…Dicyanoargentates(I) have been known for many years; lithium dicyanoargentate was prepared as early as 1921 (Meyer, 1921;Perret & Perrot, 1932;Jones, 1963;Rossmanith, 1965). Complexes of rubidium and caesium dicyanoargentates with 18-crown-6 were synthesized and structural details were reported a few years ago (Manskaya et al, 1998).…”

9-Aza steroids. III. Synthesis of some 2-cyclopentylquinolines as models for rings A, B, and D

“…The combined acid extracts were neutralized (Na2C03) and extracted with ether. The residue from the dried ethereal extracts was distilled, giving quinaldine (23.4 g), ethyl 2-quinolylacetate (18.6 g, 17%), bp 130-135°( 0.2 mm), and diethyl 2-quinolylmalonate (12) (25.6 g, 18%), bp 170-175°( 0.2 mm). The malonate 12 solidified on standing and was crystallized from petroleum ether as yellow needles: mp 72-73°( lit.7 mp 73-74°); ir 1630 cm"1; nmr (CCh) 1.28, 1.31 (overlapping t, 6, OCHCH), 4.24 (q, 4, OCHCH), 7-8.2 (m, 6, aromatic H); some specimens showed a sharp peak at 5.05, less than 1 H, due to tautomer; nmr (TFA) 1.45 (t, 6, OCHCH), 4.55 (q, 4, OCHCH), 5.75 [s, 1, CH-(C02Et)2], 8.0-8.6 (m, 5), and 9.28 (d, 1, / = 8 Hz, quinoline 4 H).…”

“…The malonate 12 was converted directly into ethyl 2-quinolylmalonate by a procedure described by Breslow26 for another substituted malonate. Decarboxylation of the half-ester occurred at 120°: yield 88%.…”

“…Diethyl 1,2,3,4-Tetrahydroquinolylidenemalonate ( 18). -The malonate 12 (2.2 g) in glacial AcOH (930 ml) was hydrogenated over Adams' catalyst at ambient temperature and pressure until uptake ceased. Evaporation, treatment of the residue with aqueous NaHCOs and ether, filtration, and evaporation of the dried ether solution gave a yellow solid, crystallized from petroleum ether as yellow plates (2 g, 90%): mp 40-41°; ir y™<" 1688, 1648, 1250, and 747 cm-'; nmr (CC14) 1.32 (¿, 6, OCHCH), 2.82 (s, 4), 4.22 (q, 4, OCHCH), and 6.7-7.3 (m, 4, aromatic); nmr (TFA) 1.1 (¿, 6), 2.6-7.3 (m, 4), 3.9-4.6 [m, 5, includes CH(C02Et)2], and 7.1 (broadened s).…”

Isolation of organomercury(II) azides stabilized by intramolecular coordination

“…Due to toxicity and difficulties in handling the mercury compounds, very few organomercury azides are reported. Further the, examples of organomercury azides known in literature were poorly characterized [14]. The first example of mercury azide (Hg 2 N 3 ) 2 was synthesized by Curtius in 1890 by reacting aqueous solutions of mercury(I) salts with alkali metal azides, or by the reaction of the free acid HN 3 with elemental mercury [14b].…”