Alcohol of crystallization

Anhydrous magnesium chloride is soluble in lower alcohols. In 100 g of methanol, its solubiUty is 15.5 g at 0°C and 20.4 g at 60°C. In ethanol, the solubihty is 3.61 g at 0°C and 15.89 g at 60°C. Upon cooling, anhydrous MgCl2 forms addition compounds with alcohols of crystallization such as magnesium chloride hexamethanolate [57467-93-0]andmagnesium chloride hexaethanolate [16693-00-8]Both of these alcoholates are deflquescent. 

In contrast to the azaquinones 1 and 3, there is no literature report on the isomeric azaquinone 2. Reported hydroxy azaquinone 17 obtained by oxidation of 2,3,4-pyridinetriol can be considered to be its 2,3-dioxo-4-hydroxy tautomer (Scheme 5) (1883JPR257). In addition, this compound was identified only as its solvate with the alcohol of crystallization, which suggests the possibility of structure 18 instead [73AG(E)139]. 

Anhydrous calcium chloride tends to form alcohols of crystallization, so you really can t use it to dry alcohols. 

This appeared to be supported by the findings of Ray and Palinchak [55] who resolved 9-nitro-2-benzoylfluorene with brucine. The brucine salt contained alcohol of crystallization and could probably be represented by the formula V ... 

Alcohol of Crystallization.—One more reaction or property of alcohol which shows its similarity to water and which might, indeed, be much more conclusive if we understood more thoroughly the way water itself acts, is that alcohol like water forms crystalline compounds with certain anhydrous substances. In case of water we term it water of crystallizationj so we may call its analogue alcohol of crystallization. Calcium chloride, CaCh, forms crystals containing alcohol of crystallization. 

Silver [7440-22-4]—The coloi additive silvei (EEC No. E 174) is a crystaUine powdei of high purity silver prepared by die reaction of silver nitrate with ferrous sulfate in the presence of nitric, phosphoric, and sulfuric acids. Poly(vinyl alcohol) is used to prevent the agglomeration of crystals and the formation of amorphous silver. 

The alcohol may be distilled from the mother liquor of the recrystallization. The residue from this distillation may be added to the mother liquor of the first crystallization, which is then concentrated to the crystallization point. The crop of crystals thus obtained will usually require double recrystallization. Alcohol recovered from the first mother liquor will contain too much volatile oil of nutmeg to be used for other purposes. 

In a 3-I. round-bottomed flask are placed 500 cc. (400 g., 8.7 moles) of absolute alcohol which has been saturated in the cold with hydrochloric acid gas (Note i), 870 cc. (6S0 g., 20 moles) of 96 per cent alcohol (Note 2) and 70 g. (1.03 moles) of methyleneaminoacetonitrile (Note 3). This mixture is refluxed on a steam bath for three hours (Note 4). During the refluxing, ammonium chloride separates. After the reaction is complete, the hot alcohol solution is filtered with suction and the filtrate cooled, thus allowing the glycine ester hydrochloride to separate out in fine white needles. The product is filtered with suction, sucked as dry as possible on the filter, and then allowed to dry in the air. The yield is about no g. The alcohol from the filtrate is distilled (Note 5) until about one-third of its volume is left and again cooled and a second crop of crystals is obtained. The total yield of product, m.p. 142-143, varies from 125 to 129 g. (89-91 per cent of the theoretical amount). If a very pure product is desired, it may be recrystallized from absolute alcohol. 

The alcoholic filtrate is evaporated to 50 cc., and 50 g. of barium hydroxide and 150 cc. of distilled water are added (Note 4). The mixture is refluxed for two hours and the excess barium hydroxide is precipitated with carbon dioxide. The barium carbonate is removed by filtration and washed with hot distilled water. A slight excess of sulfuric acid is added to the filtrate to liberate the amino acid from its barium salt, and an excess of barium carbonate is added to remove sulfate ion. The mixture is digested on the steam bath until effervescence ceases, and it is then filtered and the precipitate is washed with hot distilled water. The filtrate and washings are concentrated on the steam bath to a volume of 100 cc., decolorized with i g. of active carbon, filtered, and concentrated to the point of crystallization (about 25 cc.). The amino acid is precipitated by the addition of 150 cc. of absolute alcohol and the product is collected and washed with absolute alcohol. 

Five parts of the terpene, 7 of amyl nitrite, and 12 of glacial acetic acid are mixed and cooled with ice and salt, and a mixture of 6 parts of hydrochloric acid and 6 parts of glacial acetic acid added in small quantities at a time. Five parts of alcohol are then added and the mixture allowed to stand in a freezing mixture for a itime. A mass of crystals separates, which consists of the crude nitrosochlorides. This is filtered off and washed with alcohol. When perfectly dry 100 grams of the crystals are digested with 200 c.c. of chloroform for a few moments and at once filtered. The chloroform dissolves a-nitrosochloride, which is precipitated by the addition of excess of methyl alcohol. The crude compound is filtered off, dried and digested with anhydrous ether for... 

Baker and Smith have isolated an alcohol of the formula C,oH,gO from the cajuput oil, distilled from the leaves of Melaleuca uncinata. The alcohol, which is probably an open-chain compound, forms snow-white crystals, melting at 72 5°, and having a specific rotation + Sfi fifi . 

Terpine hydrate, CioHig(OH)3 + HjO, is a crystalline alcohol resulting from the action of dilute mineral acids on either pinene or limonene. It can be prepared by several different methods, of W hich the following is typical A mixture of 8 parts of oil or turpentine, 2 parts of alcohol, and 2 parts of nitric acid of specific gravity 1 255 IS allowed to stand for several days in a flat basin. After standing for a few days the mother liquor is poured off from the crystals of terpine hydrate, and neutralised with an alkali, after which a second crop of crystals is obtained. 

Menthol, Cj Hj OH, is the characteristic alcohol of oil of peppermint, from which it separates in fine crystals on cooling. It also results from the reduction of the corresponding ketone, menthone, Cj HigO, and. also of pulegone, CioHigO. ... 

The nitrile may best be saponified with methyl alcoholic potash while heating to 190° to 200°C with application of pressure. After the methyl alcohol has evaporated the salt is introduced into water and by the addition of dilute mineral acid until the alkaline reaction to phenolphthalein has just disappeared, the amphoteric 1-methyl-4-phenyl-piperidine-4-carbOxylic acid is precipitated while hot in the form of a colorless, coarsely crystalline powder. When dried On the water bath the acid still contains 1 mol of crystal water which is lost only at a raised temperature. The acid melts at 299°C. Reaction with ethanol yields the ester melting at 30°C and subsequent reaction with HCI gives the hydrochloride melting at 187° to 188°C. 

Cysteine is first dissolved in distilled water which has been freed of oxygen by boiling. Formaldehyde of 30% (w/v) concentration is added while stirring and the temperature of the mixture rises, while the thiazolidine carboxylic acid begins crystallizing. The stirring is continued for 2 hours after which ethyl alcohol of 95% (w/v) concentration Is added to induce further crystallization. The mixture is left to stand for 24 hours at 4°C. The mixture is then filtered with retention of a crude product, which is purified by recrystallization from boiling distilled water. The crystals are then dried at about 40°C. The free acid is then converted to the sodium salt with NaOH. 

The highest fixed nitrogen-containing fertilizer 46.7 wt %, urea is a white solid that is soluble in water and alcohol. It is usually sold in the form of crystals, prills, flakes, or granules. Urea is an active compound that reacts with many reagents. It forms adducts and clathrates with many... 

Since the alcohol has a relatively high solubility in petroleum ether, the yield from the crystallization depends on the volume of solvent used. However, by concentrating the mother liquor the overall yield from the first and second crops of crystals varies from 74% to 94%. 

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