Wako Pure Chemical Industries Ltd

Polymerisation Initiators, Product information BuUetiu, Wako Pure Chemical Industries, LTD. 

Jptt Kokai Tokkyo Koho JP62,289,574 (Dec. 16, 1987), M. Tanaka, T. Miyagawa, and H. Fuji (to Wako Pure Chemicals Industries, Ltd.). 

The checkers obtained phosphorus oxychloride from Wako Pure Chemical Industries, Ltd., Japan and distilled it prior to use. 

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 solvents and reagents without further purification. The yield of 2-hydroxyimino-2-phenylacetonitrile was 76% when the checkers used technical-grade benzyl cyanide purchased from Wako Pure Chemical Industries, Ltd., Osaka, Japan. The yield was improved to 81% with distilled material, b.p. 75-77° (3 mm.). Benzyl cyanide is also available from Aldrich Chemical Company, Inc. 

Anhydrous sodium sulfate, hydrochloric acid (36%), sodium chloride, special grade Silica gel, Wakogel C-100, adjust water content to 6.5% with distilled water (Wako Pure Chemical Industries, Ltd)... 

Methanol, ethanol, acetonitrile, benzene, trifluoroacetic anhydride, triethylamine, distilled water reagent grade (Wako Pure Chemical Industries, Ltd, Japan) Methanol, distilled water specially prepared reagent for HPLC (Wako Pure Chemical Industries, Ltd, Japan)... 

Methanol, n-hexane, ethyl acetate, distilled water, sodium chloride, sodium sulfate, reagent grade for residue analysis (Wako Pure Chemical Industries, Ltd, Japan) Acetonitrile, methanol, distilled water, reagent grade for high-performance liquid chromatography... 

R)-(+)-1,1 -Bi-2-naphthol is purchased from Wako Pure Chemical Industries Ltd. or Aldrich Chemical Company, Inc. 

Poly(diallydimethylammonium chloride) (PDDA) was purchased from Aldrich Chemical Co. 2-Morpholinoethanesulfonic acid (MES) was from Wako Pure Chemical Industries Ltd. Poly(butylviologen) (PBV), shown in Scheme 1, was synthesized according to literature method and checked by HNMR [7], Ultrapure water (18.3 M l) was prepared with a Milli-Q filtration unit of Millipore Corp. 

The submitter used diisopropylamine from Aldrich Chemical Co., and the checkers used diisopropylamine from Wako Pure Chemical Industries Ltd. (Japan). It was distilled from calcium hydride before use. 

The submitter used a 1.24M solution of n-butyllithium in pentane obtained from Foot Mineral Co., and the checkers used a 1.45M solution of w-butyllithium in hexane obtained from Wako Pure Chemical Industries Ltd. (Japan). The nominal titer of active alkyl on the bottle agreed well with the value found by titration2 with 0.S0M (submitter) or 0.50JJ (checkers) solution of 2-butanol in xylene using 1,10-phenan-throline as indicator. 

Zinc chloride available from Mai 1 inckrodt, Inc., was flame-dried under a slow stream of nitrogen. The checkers used the material from Wako Pure Chemical Industries, Ltd., after heating under vacuum (1 mm). 

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