Zinc chloride, anhydrous

Zinc, cyclopropane from 1,3-dichloropropane, 51, 58 Zinc, activated, 53, 88 Zinc chloride, anhydrous, ethereal solution, preparation of, 54, 54... 

Esterification is effected in the cold in presence of alkali or by heating the alcohol and anhydride together, usually in presence of a dehydrating agent—e.g., fused zinc chloride, anhydrous sodium acetate, etc. Preparation 204.—Mannitol Hexacetate. 

SYNS BUTTER of ZINC CHLORURE de ZINC (FRENCH) ZINC BUTTER ZINC CHLORIDE (ACGIH, OSHA) ZINC CHLORIDE, anhydrous (UN 2331) (DOT) ZINC CHLORIDE, solution (UN 1840) (DOT) ZINC (CHLORURE de) (FRENCH) ZINC DICHLORIDE ZINC MURIATE, solution (DOT) ZINCO (CLORURO di) (ITALIAN) ZINKCHLORID (GERMAN) ZINKCHLORIDE (DUTCH)... 

Zinc chloride, anhydrous Magnesium chloride, anhydrous Iron(II) sulfate... 

ZINC CHLORIDE,ANHYDROUS,TECH.GR. MOISTORE SENSITIVE... 

Synonyms Butter of zinc Zinc butter Zinc chloride anhydrous Zinc chloride fume Zinc chloride, solution... 

Vinyl Pyridines. inhibited 3073 57 Zinc Chloride, anhydrous 2331 60... 

AICI3 6H2O (hydrated aluminum chloride), 250 g ZnCn.2 (zinc chloride) (anhydrous) 30-60 1-6 min ... 

C (decomp.). Prepared by reacting ketene with methanol under carefully controlled conditions in the presence of anhydrous zinc chloride. This highly reactive compound has many synthetic uses, chiefly for adding the... 

For complete acetylation of polyhydric compounds, such as glucose (p. 141) and mannitol (p. I42), even undiluted acetic anhydride is insufficient, and a catalyst must also be employed. In such cases, the addition of zinc chloride or anhydrous sodium acetate to the acetic anhydride usually induces complete acetylation. ... 

Carry out this preparation precisely as described for the a-compound, but instead of zinc chloride add 2 5 g. of anhydrous powdered sodium acetate (preparation, p. 116) to the acetic anhydride. When this mixture has been heated on the water-bath for 5 minutes, and the greater part of the acetate has dissolved, add the 5 g. of powdered glucose. After heating for I hour, pour into cold water as before. The viscous oil crystallises more readily than that obtained in the preparation of the a-compound. Filter the solid material at the pump, breaking up any lumps as before, wash thoroughly with water and drain. (Yield of crude product, io o-io 5 g.). Recrystallise from rectified spirit until the pure -pentacetylglucose is obtained as colourless crystals, m.p- 130-131° again two recrystallisations are usually sufficient for this purpose. 

Required Resorcinol, 5 g. acetonitrile, 3 5 ml. zinc chloride, 2 g., anhydrous ether, 25... 

Required Aniline, 24 ml. nitrobenzene, 13 ml. anhydrous glycerol, 62 ml. sulphuric acid, 36 ml. zinc chloride, 23 g. 

Pure pyridine may be prepared from technical coal-tar pyridine in the following manner. The technical pyridine is first dried over solid sodium hydroxide, distilled through an efficient fractionating column, and the fraction, b.p. 114 116° collected. Four hundred ml. of the redistilled p)rridine are added to a reagent prepared by dissolving 340 g. of anhydrous zinc chloride in a mixture of 210 ml. of concentrated hydrochloric acid and 1 litre of absolute ethyl alcohol. A crystalline precipitate of an addition compound (probable composition 2C5H5N,ZnCl2,HCl ) separates and some heat is evolved. When cold, this is collected by suction filtration and washed with a little absolute ethyl alcohol. The yield is about 680 g. It is recrystaUised from absolute ethyl alcohol to a constant m.p. (151-8°). The base is liberated by the addition of excess of concentrated... 

Zinc cyanide. Solutions of the reactants are prepared by dis solving 100 g. of technical sodium cyanide (97-98 per cent. NaCN) in 125 ml. of water and 150 g. of anhydrous zinc chloride in the minimum volume of 50 per cent, alcohol (1). The sodium cyanide solution is added rapidly, with agitation, to the zinc chloride solution. The precipitated zinc cyanide is filtered off at the pump, drained well, washed with alcohol and then with ether. It is dried in a desiccator or in an air bath at 50°, and preserved in a tightly stoppered bottle. The yield is almost quantitative and the zinc cyanide has a purity of 95-98 per cent. (2). It has been stated that highly purified zinc cyanide does not react in the Adams modification of the Gattermann reaction (compare Section IV,12l). The product, prepared by the above method is, however, highly satisfactory. Commercial zinc cyanide may also be used. 

Lucas reageut is prepared by dissolving 68 g. (0-5 mole) of anhydrous zinc chloride (fused sticks, powder, etc.) in 62 6 g. (0 6 mole) of concentrated hydrochloric acid with cooling to avoid loss of hydrogen chloride. 

By refluxing the alcohol with a mixture of concentrated hydrochloric acid and anhydrous zinc chloride, for example ... 

After the butyl chloride fraction has been collected, change the receiver and continue the distillation untU the zinc chloride commences to crystallise. Allow to cool and stopper the flask. The anhydrous zinc chloride thus obtained may be used in another preparation and recovered repeatedly. This results in considerable economy when the preparation is conducted by a large number of students. 

Reflux a mixture of 68 g. of anhydrous zinc chloride (e.g., sticks), 40 ml. (47 -5 g.) of concentrated hydrochloric acid and 18-5 g. (23 ml.) of sec.-butyl alcohol (b.p. 99-100°) in the apparatus of Fig. 777, 25, 1 for 2 hours. Distil oflF the crude chloride untU the temperature rises to 100°. Separate the upper layer of the distillate, wash it successively with water, 5 per cent, sodium hydroxide solution and water dry with anhydrous calcium chloride. Distil through a short column or from a Claisen flask with fractionating side arm, and collect the fraction of b.p. 67-70° some high boiling point material remains in the flask. Redistil and collect the pure cc. butyl chloride at 67-69°. The yield is 15 g. 

Allyl Chloride. Comparatively poor yields are obtained by the zinc chloride - hydrochloric acid method, but the following procedure, which employs cuprous chloride as a catalyst, gives a yield of over 90 per cent. Place 100 ml. of allyl alcohol (Section 111,140), 150 ml. of concentrated hydrochloric acid and 2 g. of freshly prepared cuprous chloride (Section II,50,i one tenth scale) in a 750 ml. round-bottomed flask equipped with a reflux condenser. Cool the flask in ice and add 50 ml. of concen trated sulphuric acid dropwise through the condenser with frequent shaking of the flask. A little hydrogen chloride may be evolved towards the end of the reaction. Allow the turbid liquid to stand for 30 minutes in order to complete the separation of the allyl chloride. Remove the upper layer, wash it with twice its volume of water, and dry over anhydrous calcium chloride. Distil the allyl chloride passes over at 46-47°. 

Add 1 ml. of the alcohol-free ether to 0-1-0-15 g. of finely-powdered anhydrous zinc chloride and 0 5 g. of pure 3 5-dinitrobenzoyl chloride (Section 111,27,1) contained in a test-tube attach a small water condenser and reflux gently for 1 hour. Treat the reaction product with 10 ml. of 1-5N sodium carbonate solution, heat and stir the mixture for 1 minute upon a boiling water bath, allow to cool, and filter at the pump. Wash the precipitate with 5 ml. of 1 5N sodium carbonate solution and twice with 6 ml. of ether. Dry on a porous tile or upon a pad of filter paper. Transfer the crude ester to a test-tube and boil it with 10 ml. of chloroform or carbon tetrachloride filter the hot solution, if necessary. If the ester does not separate on cooling, evaporate to dryness on a water bath, and recrystallise the residue from 2-3 ml. of either of the above solvents. Determine the melting point of the resulting 3 5 dinitro benzoate (Section 111,27). 

CH3)3COH+CH3COCl+C H5N(CH3), CH3COOC(CH3)3+C.H5i (CH3)jHCl or from the alcohol and acetic anhj dride in the presence of a little anhydrous zinc chloride ... 

J The hexa.acetyl derivative, m.p. 121°, may be prepared as follows. Boil under reflux 1 part of mannitol with 5 parts by weight of acetic anhydride and 1 part of anhydrous sodium acetate or with a little anhydrous zinc chloride for 15-20 minutes, pour into excess of water, stir the mixture until the oil has solidifled, and then recrystallise from methylated spirit. 

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