Acetone preparation

Appendix - Phenyl acetones by electrolytic oxidation. Process for 3,4-dimethoxyphenyl-acetone preparation. European Patent Application 0247526, Filed 02.12.87 to LARK S.p.a. Milan. 

In the chemical industry, simple aldehydes and ketones are produced in large quantities for use as solvents and as starting materials to prepare a host of other compounds. For example, more than 1.9 million tons per year of formaldehyde, H2C=0, is produced in the United States for use in building insulation materials and in the adhesive resins that bind particle hoard and plywood. Acetone, (CH.3)2C"0, is widely used as an industrial solvent approximately 1.2 million tons per year is produced in the United States. Formaldehyde is synthesized industrial ) by catalytic oxidation of methanol, and one method of acetone preparation involves oxidation of 2-propanol. 

Acid-FeCh in acetone (Dissolve 150 mg FeCf 6 H20 in 3 ml 0.3 N HC1 and mix with 97 ml acetone— prepare fresh before use.)... 

Sulfosalicylic acid in acetone—Dissolve 6.25 g of sulfosalicylic acid in 500 ml of acetone. Prepare on the day of the experiment. Store in a tightly stoppered bottle. 

Ninhydrin. Reacts with drugs that contain primary or secondary amines, such as amphetamine and other sympathomimetic amines. Dissolve 100 mg ninhydrin in 100 mL of acetone. Prepare fresh reagent for each test. 

Later, X-ray diagrams given by nitrocelluloses with acetone prepared after the Desmaroux method by absorbing acetone from castor oil solutions, were examined by Mathieu [34]. The spacing of the plane Af (101) (Fig. 84, Table 38) was 7.25 A for trinitrocellulose, and less than 7 A for nitrocellulose of 11.6% N. However, the distance in both types of nitrocellulose is increased considerably as acetone is absorbed, approaching 11 A when the acetone to nitrocellulose mole ratio is 1 1, i.e. when one molecule of CH3COCH3 corresponds to three ONOj groups. 

Sodium enolates of ketones have been prepared by reaction of these ketones with NaNH2. For example, the alkylation of the sodium enolate of cyclohexanone by allylbromide (Fig. 2) leads to 2-allylcyclohexanone accompanied by a little of the dialkylated product (ref. 14). Dimethyl ethynyl carbinol was obtained by reaction of the enolate of acetone (prepared by reaction of solid NaNH2 in ether) with acetylene. Although a prepared ketone enolate is used, this reaction can also be considered as an aldolisation reaction of the acetylide with acetone (ref. 15). Hauser and coll, react sodioenolates of ketones prepared in ether (ref. 16) with acid chlorides (Fig. 2). 

The acetone prepared in this way contains impurities from which it may be freed by treatment with acid sodium sulphite. Pure acetone is liberated from the crystalline addition-product formed, by heating the latter with a solution of sodium carbonate. 

Silane slide coating solution 2% (v/v) 3-aminopropyltriethoxysilane (Sigma, cat. no. A3648) in acetone. Prepare fresh just before use (see Section 3.2.). 

In the case of relatively low-melting solids it is also possible to prepare a thin film by melting and squeezing the sample between two windows. Thin films of nonvolatile liquids or solids can be deposited on the window by solvent evaporation. The sample is first dissolved in a volatile solvent A few drops of the solution are placed on the window. After evaporation of the solvent, a thin film of sample is obtained on the window. The windows can usually be cleaned using carefully dried methylene chloride or acetone. Preparing a thin film from solution or sohdification from the melt are methods well suited to the examination of amorphous materials, such as waxes or soft resins. 

A fresh solution (50 mL) of isolated DDO (0.06-0.08 M in acetone), prepared as reported, is diluted with an equal volume of cold water (0-5 °C) and extracted in a chilled separatory funnel with four 10 mL portions of cold CH2CI2, CHCI3, or CCU... 

Aminopyrimidyl-acetaldehydes and -acetones prepared by hydrolysis of their acetals cyclize spontaneously to pyrrolo[2,3-d]pyrimidines.—E 4-Amino-5-(2,2-diethoxyethyl)-2,6-dihydroxy pyrimidine shaken 24 hrs. with 1.5 equivalents of 0.2 N HCl 2,4-dihydroxypyrrolo[2,3-d]-pyrimidine. Y 93%. F. e. and method s. J. Davoll, Soc. I960, 131. 

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