Diethyl ether mass spectrum

Purify the crude product by chromatography (diethyl ether hexane, 1 8) and the pure alcohol is obtained with 77% yield. Identify it by 1H and 13C NMR, IR, elemental analysis, and mass spectrum. 

The mass spectrum of diethyl ether appears in Figure 14-5. The four most abundant ions correspond to the molecular ion, loss of an ethyl group, a cleavage, and loss of an ethylene molecule combined with a cleavage. All these modes of cleavage form resonance-stabilized oxonium ions. 

After the treatment of 3a with H2O2 followed by the addition of an excess of diethyl ether, 3b could successfully be isolated. The positive-ion coldspray ionization mass spectrum of the isolated 3b showed a most intense parent ion peak centered at m/z = 3654.8 with an isotopic distribution that agreed with the calculated pattern of [(TBA)5SiWio032(02)2] - All these results show that the two 0x0 groups (O ) are replaced by two peroxo groups (C ) on the divacant lacunary site with retention of the y-Keggin framework (Eq. 4.2). 

The phenylethynyl complex forms lemon-yellow crystals mp 205° (dec.) (checker, 200-205°), which are insoluble in light petroleum, diethyl ether, methanol, and ethanol but soluble in dichloromethane, chloroform, and tetra-hydrofuran. The infrared spectrum has a sharp v(C=C) band at 2068 cm"1, and the H nmr spectrum contains resonances at r 2.52m, 2.90m (35H, Ph) and 5.67s (5H, CSHS). The mass spectrum contains a parent ion centered on m/e 792 (calcd. for 102Ru, 792). 

A gas-chromatographic analytical procedure is available (Ref 13). Mass spectra have been published for all the isomers (Ref 10). In all cases, initial reaction in obtaining the spectrum involves interaction between the methyl group and an adjacent nitro group, except in the case of the 3,4,5-isomer, which lacks this requirement. The isomers can be separated from each other by adsorption chromatography over silica gel (Ref 16), or by treatment of the mixt with aq urea (Ref 14). They are poorly soluble in water, but easily soluble in acetone, diethyl ether, and aromatic hydrocarbons. The 2,4,5-isomer can be purified by recrystn from abs ethanol, all of... 

Ethylidynetrinickel cluster 1 (NiCp)3CCH3 was prepared for the first time from the reaction of nickelocene with methyllithium, in diethyl ether and THF. 1 sublimes at 60 °C (0.001 Torr), melts without decomposition at 158-160 °C, oxidizes easily in air but does not hydrolyze in water. The mass spectrum shows a parent peak at m/z 396 ( Ni). The C NMR of 1 established the presence of the ethylidyne carbon atom at S 289.3 (s). The molecular structure of 1 is shown on Fig. 1. The nickel framework is best described as an isoceles triangle. The C2 atom of the apical methylidyne group is tilted slightly towards the Ni 1 atom. 

Diethyl phosphorofluoridate is a colorless liquid that can be readily distilled under reduced pressure. It is very soluble in benzene, hexane, and diethyl ether. It is stable for long periods under anhydrous conditions. The mass spectrum gives a molecular ion at mie 155. P NMR (H3PO4) 8 -9.52 (d, 7p F = 964 Hz) F NMR (CCI3F) < ) -81.46 (d). 

Although many of the products of the reaction were very polar, as shown by HPLC and thin-layer chromatography, we were able to determine some of the products by extracting the aqueous solution of a preparative-scale reaction done at pH 8 with diethyl ether and analyzing the extract by gas chromatography-mass spectroscopy (GC-MS). The principal ether-soluble product was 2-hydroxy-l,4-naphthoquinone (lawsone, 4). The mass spectrum of lawsone was sufficiently characteristic to distinguish it clearly from other hydroxynaphthoquinone isomers such as Juglone (11). Lawsone has also been reported previously as a product of photolysis of 1-naphthol in alkaline solution (12). 

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