Alcoholic Ferric Chloride

The condensation is carried out in the usual manner in chloroform solution. The product separates from alcohol with 1 5 molecules of solvent of crystallisation, which can be removed at 110° C. It gives the iodoform test with iodine in aqueous sodium hydroxide. At 260° to 265° C. it decomposes. It is insoluble in w ater, but dissolves in hot alcohol or aqueous sodium hydroxide. Alcoholic ferric chloride gives a faint olive-green tint concentrated sulphuric acid gives no coloration in the cold, but on warming an olive-green tint appears, changing to deep red. The chloride may be converted to the oodde in the usual manner. 

Tellurium 3-ethylacetylacetone di-iodide, (C5H502.C2H5) Tel2, crystallises from ethyl alcohol as light scarlet crystals. In powdered form and in alcoholic solution it is orange in colour. It gives no coloration with aquo-alcoholic ferric chloride. It sinters and blackens at 149° C., and decomposes with intumescence at 176° C. 

Tellurium dibutyrylmethane trichloride (Formula III).—This is isolated when the final mother-liquors from the dichloride are concentrated and cooled to 0° C. It yields large tabular crystals, melting and blackening at 87° to 88° C. Unlike the dichloride it develops a blood-red coloration with aquo-alcoholic ferric chloride. It is decomposed by moisture, and is very soluble in chloroform. 

Alcohol Content of Ethyl Oxyhydrate (Flavor Chemicals), 585 Alcoholic Ferric Chloride TS, 852 Alcoholic Potassium Hydroxide, 0.5 N, 854... 

The condensation of a, dicarbonyl compounds (49) with aj3-diamino compounds (50), which proceeds through the dihydropyrazine (51), has been much used for the synthesis of alkyl- and arylpyrazines (52). These reactions are usually carried out in methanol, ethanol, or ether in the presence of sodium or potassium hydroxide. The dihydropyrazines may be isolated, or oxidized directly to the pyrazine. Dehydrogenating agents that have been employed include oxygen in aqueous alkali (329), air in the presence of potassium hydroxide (330), sodium amylate in amyl alcohol (330a), alcoholic ferric chloride (24), and copper chromite catalyst at 300° (331) (see also Section 1). Pyrazines prepared by this method and modifications described below are listed in Table II.8 (2, 6, 24, 60, 80,195, 329-382) and some additional data are provided in Sections VI. 1 A, VlII.lA(l), and IX.4A(1). 

The early work on this compound was confused by Pschorr s failure to recognize its phenolic nature. He noted the alkali-soluble nature of the methiodide and the production of a mono-acetyl derivative, but concluded, on account of the apparent insolubility of the parent base in alkali, that fission of the cyclic ether fink occurred during the reactions of the base with acetic anhydride and methyl iodide [7]. That /3-ethylthiocodide is indeed a phenol was demonstrated by Morris and Small [3] it gives coloured solutions with alcoholic ferric chloride and readily couples with diazonium salts in alkaline solution to give red dyes moreover it is soluble in alkali, though not readily so, being a very weakly acidic phenol. 

Gardenin A, C .H, 09, S-hydroxy-6,7,8 trimetfioty.2 3,4,5.trimethoxyphenyl).4H.l.benzopyran-4 >ne. R — R = OCH,. Golden yellow needles from ethanol, rap 162-163. Sol in alcohol, chloroform. All the gardenins give a green color with alcoholic ferric chloride. 

In a large test tube, prepare a mixture consisting of 2 ml of 1 M hydroxylamine hydrochloride in propylene glycol, 30-50 mg of the compound that has been dissolved in a minimum amount of propylene glycol, and 1 ml of 1 A/f potassium hydroxide. Heat the mixture to boiling for 2 min and then cool it to room temperature. Add 0.5-1.0 ml of a 0.5 M alcoholic ferric chloride solution. A red-to-violet color is a positive test. Yellow colors are negative, and brown colors and precipitates are neither positive nor negative. 

Bisnorargemonine, C19H21O4N (mp 254°) from Argemone and Esch-scholtzia species has two phenolic hydroxyls and on methylation with diazomethane is converted to argemonine. Its hydroxyls are vicinal as indicated by its NMR-spectrum and by the intense color that it gives with alcoholic ferric chloride, and therefore its structure is known (87). 

These directions are those of Nij tingale, Taylor, and Smelser (reference 42). A smaller yield (50-55%) is obtained unth aluminum chloride as a catal3rst (Fieser, "Experiments in Organic Chemistry," 2nd ed... D. C. Heath and Co., New York, 1941, p. 179). The same situation holds for t-butyl alcohol, ferric chloride giving better yields than aluminum chloride [Potts and Dodson, J, Am, Chetn. Soc., 61,2553 (1939)]. 

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