The amount of the particular zinc or zirconium compound added to the aqueous bromide solution is also not particularly crucial, and may vary over a wide range. © Copyright 2020 Alfa Aesar, Thermo Fisher Scientific. But as mentioned above, the actual range of water content in the dried product will probably be somewhat lower. Thus, in the case of the zinc derivatives, the generalized formula will be: [Al2 (OH)6-x Brx ](y/2) Zn Clz Br2-z. lack of gelation tendencies) after one week at ambient temperatures. After overnight stirring, 68 gm of the solution was dried in a rotary vacuum evaporator at 30°C. The product dissolved in anhydrous SDA-40 in about 0.4 hour to form a 30% solution with a CCl4 compatibility of 251 cc. In the alternative, the zirconium compounds can be made by dissolution of commercially available zirconium carbonate paste (carbonated hydrous zirconia) in the appropriate amount of the halogen acid. The composition must be compatible with the halogenated hydrocarbons which are conventionally employed as propellants in aerosol antiperspirant sprays; and. 3,405,153. In many of the reactions, organozinc compounds appear as intermediates, and a few popular examples are: the Reformatsky reaction, Simmons-Smith reaction, Negishi coupling reaction, Frankland–Duppa reaction, Fukuyama coupling reaction, and Barbier reaction. The product dissolved in anhydrous SDA-40 in about an hour to form a 30% solution with a CCl4 compatibility of 190 cc. 1981). All Rights Reserved. To 60.5 gm 50% basic aluminum bromide (11.1% Al) was added 26.4 gm of zirconyl hydroxychloride (20.2% Zr) giving an Al/Zr ratio of 6.0:1. and about 15 mm Hg. The above and other objects are achieved by the complexes of the present invention which are prepared by providing an aqueous solution of five-sixths basic aluminum bromide; mixing with the aqueous solution a compound selected from the group consisting of zinc chloride, zinc bromide, zirconyl chloride, zirconyl bromide, zirconyl hydroxychloride, zirconyl hydroxybromide, and mixtures of these compounds; and drying the resulting mixture to produce the complex in the form of a substantially friable solid. However, to date there is no significant evidence that heating or standing adversely affects any of the dried products. For the determination of Zinc carnosine, the proposed HPLC method was found to be superior due to high percentage recovery which shows that the method was free from interference of excipients used in the formulations. Thus, in order to be commercially acceptable for use in present day aerosol antiperspirant compositions, it is generally necessary that the astringent compositions meet the following requirements: 1. Samples should therefore be protected from sources of moisture, including the water vapor present in ambient air. The zinc halides may also be easily and relatively cheaply prepared by dissolution of zinc or zinc oxide in hydrochloric acid or hydrobromic acid. The solution was dried in a rotary vacuum evaporator at 30°C. and about 15 mm Hg. For example, virtually all of the products are soluble in anhydrous (SDA-40) alcohol within about one hour or less to the extent of at least about 30 weight percent. No. Thus, the zirconium complexes generally have CCl4 compatibilities in the range of about 150 to 250 or more, while the zinc complexes generally have CCl4 compatibilities of about 100 to 200. 2,906,668 for "ZIRCONYL AND ALUMINUM HALOHYDROXY COMPLEX" issued to Stewart M. Beekman, which discloses aqueous solution complexes of zirconyl halides with aluminum hydroxyhalides and a method for maintaining a high solution pH and preventing gelling. Nos. Thus, the zirconyl chloride or bromide complexes, which are the most compatible, have a pH range of about 0.9 to 1.4; the zirconyl hydroxychlorides or hydroxybromides have a pH range from about 1.5 to 2.5; and the zinc chlorides or bromides, which have the lowest compatibility, have a pH range from about 2.4 to 2.6. 2,814,584 and 2,814,585 for "BUFFERED ANTIPERSPIRANT COMPOSITIONS" issued to Edwin William Daley, which disclose aqueous solutions of zirconium and/or hafnium salts which are buffered with basic aluminum halides or nitrates and amino acids to render the solutions safe for antiperspirant usage. 3. Analysis: 16.1% Al, 5.7% Zr, 35.1% Br, 21.3% H2 O by Karl Fischer. and about 15 mm Hg. 227 gm of zirconyl hydroxybromide (21.7% Zr) was added to 1,336 gm of 50% basic aluminum bromide (10.9% Al) giving an Al/Zr ratio of 10.0:1. However, in the presence of aluminum, the assays for zinc and zirconium are somewhat uncertain, and therefore Karl Fischer values are used throughout the application rather than calculated values. Analysis: 17.3% Al, 6.2% Zr, 31.1% Br, 18.7% H2 O by Karl Fischer. & Terms of Use. After overnight stirring, the solution was dried in a rotary vacuum evaporator at 30°C. Another example is U.S. Pat. 1993, 93, 2117-2188 and Kim, S.-H.; Rieke, R. D. “Recent Advance in Heterocyclic Organozinc and Organomanganese Compounds; Direct Synthetic Routes and Application in Organic Synthesis”.