NOTES 411with barely detectable traces of CdCr04-I1 and the other unidentified phase. There is evidence that such an amorphous phase is also present in quench products obtained from lower temperature runs (250-450') where CdCr04-I1 is the major crystalline phase. All the X-ray patterns of CdCr04-II were of lower intensity than would be expected for the amount of powder used. Moreover, a prominent broad highintensity region a t low 28 values was always present, again suggesting the presence of an amorphous phase. Further evidence for an amorphous phase is given by infrared data.Infrared spectra were taken for (a) a sample rich in CdCr04-II and (b) a nearly amorphous CdCr04 specimen. The spectra are very similar to each other and also resemble the spectrum of a-CdCr04.' The frequencies (in cm-I) are compared below. The data CdCrO4-11-containing sample Amorphous a-CdCrOa 915 + 898 912 915 855 855 865 802 790 805

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out under an atmosphere of dry nitrogen.General Procedure. All of the experiments were carried out in a similar manner. The following is a typical procedure: Hexachlorocyclotriphosphazene (5.0 g, 0.014 mol) was dissolved in THF (150 mL). The methyllithium solution (22.4 mL, 0.028 mol) was slowly added over a period of ~20 min. The reaction mixture was allowed to stir overnight. Removal of the solvent under vacuum and filtration of the products dissolved in CH2C12 through neutral alumina gave the cyclic products. The yields are listed in Table I. For reactions involving TMEDA, the phosphazene (5.0 g, 0.014 mol) and TMEDA (8.45 mL, 0.056 mol) were first dissolved in the solvent and then the organometallic reagent was added as before. For reactions involving ethyl bromide, the phosphazene (5.0 g, 0.010 mol) and ethyl bromide (2.09 mL, 0.028 mol) were dissolved in the solvent and the above procedure repeated.Acid Hydrolysis. The "ring-cleaved" products from the above reactions were all hydrolyzed in the same manner. The following is a typical procedue: A 1.0-g sample of the material was placed in a glass ampule with ethanol (30 mL) and 2 M HC1 (30 mL). The ampule was then cooled to -196 °C, evacuated, and sealed and was then heated at 150 °C for 24 h. After this time, the ampule was allowed to cool at room temperature and opened, and the solvent was removed in vacuo. Sublimation of the solid residue at 80 °C (0.5 mm) yielded ~0.1 g of (CH3)3P=0 (identified by its mass spectrum and 31P NMR). Extraction of the sublimator residue with toluene gave a mixture that proved to be (CH3)2P(0)OH, CH3P(0)(OH)2, and H3P04 (identified by mass spectrometry and 31P NMR).

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Die elektrochemische Synthese von Benzindolen aus Aminonaphthalenen in Gegenwart von Arsoniumyliden Die elektrochemische Synthese von 2‐Aryl‐1 H‐benz[g]indolen (3a–c) und 2‐Aryl‐3 H‐benz[e]indolen (4a–c) aus methanolischer Lösung von 1‐ oder 2‐Aminonaphthalenen in Gegenwart von kathodisch gebildeten Arsoniumyliden (2a–c) wird beschrieben. Die optimalen Synthesebedingungen werden diskutiert.