Mallinckrodt Chemical Works

Wallingford, V.H. U.S. Patent 2 611,786 September 23,1952 assigned to Mallinckrodt Chemical Works. 

Xylene (analytical reagent grade) from Mallinckrodt Chemical Works was distilled from sodium before use. 

Commercial C.p. chloroplatinic acid varies somewhat in its purity. In this work that from the Mallinckrodt Chemical Works, St. Louis, was used and gave very satisfactory results. Since small amounts of impurities in the catalyst are important factors in the rate of reduction of certain types of compounds, this question of impurities in the chloroplatinic acid must be taken into account (Note 13). In a large proportion of the reductions studied, platinum oxide prepared from the chloroplatinic acid mentioned gave as good results as that from spectroscopically pure chloroplatinic acid made according to the directions of Wichers.1... 

Benzocaine was purchased from Mallinckrodt Chemical Works and was recrvstallized from absolute ethanol prior to use to give material of m.p. 91-92°. 

The submitters used the following reagents as supplied iodine, ether, and sodium acetate from Mallinckrodt Chemical Works, dinitrogen tetroxide from Matheson Gas Company, and ethyl acrylate from Aldrich Chemical Company, inc. The checkers obtained dinitrogen tetroxide from Matheson Gas Company and the other reagents from Wako Pure Chemical Industries, Ltd., Japan. 

The submitters used reagent-grade acetonitrile (Mallinckrodt Chemical Works) dried prior to use by storage over Matheson Linde type 4A molecular sieves. The checkers used reagent-grade acetonitrile obtained from Ishizu Pharmaceutical Company, Japan, dried prior to use by storage over 4A molecular sieves obtained from Nakarai Chemicals, Ltd., Japan. 

OH) (purchased from Fisher Scientific Company) and Amberlite IRA-400 (purchased from Mallinckrodt Chemical Works) were found to be satisfactory. Chloride-form resins must be converted to the hydroxide form before use, as described below (Note 7). 

Tetrahydrofuran (purchased from Mallinckrodt Chemical Works) was dried by distillation from lithium aluminum hydride, and stored over Linde 4A Molecular Sieves. 

Magnesium metal turnings from Fisher Scientific Company or Mallinckrodt Chemical Works were used. Excess magnesium or incomplete formation of the Grignard must be avoided, since any... 

A 30% solution of hydrogen peroxide in water was purchased from Mallinckrodt Chemical Works. The reaction requires 2 molar equivalents of hydrogen peroxide, the first to oxidize the selenide to the selenoxide and the second to oxidize the elimination product, benzeneselenenic acid, to benzeneseleninic acid. The submitters recommend that the hydrogen peroxide solution be taken from a recently opened bottle, or titrated to verify its concentration. 

Anhydrous ethyl ether purchased from Fisher Scientific Company or Mallinckrodt Chemical Works was dried over Linde type 3A molecular sieves. The checkers degassed the solvent immediately before use by evacuating and filling the container with nitrogen three times. 

Potassium hydroxide (85% minimum assay) obtained from the Mallinckrodt Chemical Works is satisfactory. 

The submitters used practical grade anthranilic acid from Mallinckrodt Chemical Works. 

The submitters used amyl nitrite U.S.P. from Mallinckrodt Chemical Works isoamyl nitrite supplied by Matheson, Coleman and Bell is apparently the same material. They found that other alkyl nitrites (ethyl, w-butyl, 1-butvl, amyl) may be used with equal success. Subsequent to the checking of this procedure, they reported that the amount of nitrite can be reduced to a 20% molar excess. 

Zinc powder, obtainable from Mallinckrodt Chemical Works, St. Louis, Missouri, and Merck and Co., Rahway, New Jersey, is placed in a beaker and is washed consecutively and rapidly ( 10 seconds) with three 100-ml. portions of 3% hydrochloric acid, two 100-ml. portions of water, two 200-ml. portions of 2% aqueous copper sulfate (until blue color disappears), two 200-ml. portions of water, two 100-ml. portions of acetone, two 100-ml. portions of dimethylformamide, and is washed into the reaction vessel with dimethylformamide. This procedure is a modification of one described by Hennion and Sheehan.3... 

Once the cocaine has been legally produced from the coca leaf, it is exported to various countries for medicinal use, basically as a topical local anesthetic (applied to the surface, not injected, only treating a particular area). In the United States the crystalline powder is imported to pharmaceutical companies who process and package the cocaine for medical use. Merck Pharmaceutical Company and Mallinckrodt Chemical Works distribute cocaine in crystalline form (Hydrochloride Salt) in dark colored glass bottles to pharmacies and hospitals throughout the United States. Cocaine, in the alkaloid form (base drug containing no additives such as hydrochloride in the crystalline form) is rarely used for medicinal purposes. Cocaine hydrochloride crystals or flakes come in Vs, A and 1 ounce bottles from the manufacturer and has a wholesale price of approximately 20 to 25 per ounce (100% pure). 

The submitters used pentane " petroleum spirit (b.p. 25-40°) available from Hopkin Williams Ltd., Hadwell Heath, England, and anhydrous diethyl ether available from May Baker Ltd., Dagenham, England. Both solvents were each distilled over solid potassium hydroxide before use. The checkers purchased pentane from Phillips Petroleum Company and distilled it over solid potassium hydroxide. Anhydrous diethyl ether supplied by Mallinckrodt Chemical Works was used without further purification. 

A new container of anhydrous ether from Mallinckrodt Chemical Works or Merck and Co. is satisfactory. 

The submitters used anhydrous, sublimed aluminum chloride obtained from E. Merck AG, Darmstadt, Germany. The checkers used analytical reagent grade material obtained from Mallinckrodt Chemical Works. 

The submitters employed, without purification, 98% ethylenediamine obtained from Mallinckrodt Chemical Works the checkers employed material from Eastman Organic Chemicals which was redistilled (b.p. 117-118°) before use. The amount of ethylenediamine employed is sufficient to provide three equivalents of diamine for each mole of chro-mium(II) and to neutralize any acid remaining in the chro-mium(II) perchlorate solution. 

A reagent grade copper(II) sulfate pentahydrate, purchased from either Mallinckrodt Chemical Works or J. T. Baker Chemical Company, may be employed. 

Anhydrous ether available from Mallinckrodt Chemical Works can be used without further drying. 

Inc. sodium hydride (58% dispersion in mineral oil), Alfa Products, Division of the Ventron Corporation trichloroacetonitrile, Aldrich Chemical Company, Inc. xylene (a mixture of isomers, b.p. 137—144°), Mallinckrodt Chemical Works anhydrous ethyl ether, Mallinckrodt Chemical Works Silica Gel (Grade 62), Grace Davidson Chemical. The reagents used by the checkers were obtained from the following sources geraniol (98.7%), sodium hydride (58% dispersion in mineral oil), trichloroacetonitrile, and xylene (a mixture of isomers, b.p. 137-143°), Fluka AG, Chemische Fabrik, Buchs, Switzerland Silica gel (70-230 mesh ASTM), E. Merck AG, Darmstadt, Germany. 

Reagent-grade toluene employed by the submitters was obtained from Mallinckrodt Chemical Works. The checkers used reagent-grade toluene purchased from Wako Pure Chemical Industries, Ltd., and dried over molecular sieves (4 A) before use. Regarding the volume of the toluene used by the checkers, see Note 3). 

The silicic acid used for column chromatography and the Amberlite resin were Silicar CC-7 100-200 mesh purchased from Mallinckrodt Chemical Works, St. Louis, Mo. The 5% palladium on charcoal catalyst was purchased from Engelhard Industries Ltd., Newark, N. J. The tri-O-acetyl-D-glucal and the tri-O-acetyl-D-galactal (as a 70% solution in benzene) were purchased from Raylo Chemicals Limited, Edmonton, Alberta. 

Crystalline p-bromophenol and p-toluene sulfonate were obtained in reagent grade form from Eastman Kodak Company. Reagent grade phenol was obtained from Mallinckrodt Chemical Works. 

Bertsch, H.C. and Lemp, J.F. US Patent 2,848,366 August 19, 1958 assigned to Mallinckrodt Chemical Works... 

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