Preparation of 4,4'-azobis(4-cyanovaleric acid)
Abstract
Abstract PURPOSE:To obtain the titled compound in high yield, by reacting a mixture of a cyanide compound and a hydrazine with levulinic acid in the presence of a specific amount of water, adding acetone and water to the prepared concentrated aqueous solution of a hydrazo compound, oxidizing the hydrazo compound with chlorine. CONSTITUTION:A mixture of a cyanide compound and a hydrazine is brought into contact with and reacted with levulinic acid or Na levulinate in the presence of 25-200pts.wt. preferably 30-100pts. wt. based on 100pts.wt. levulinic acid or Na levulinate at 5-40 deg.C, to give a concentrated aqueous solution of a hydrazo compound. Acetone and/or water is added to the concentrated aqueous solution, then tne hydrazo compound is oxidized (preferably at <=10 deg.C) with a chlorine gas, to give the aimed compound. When the concentrated aqueous solution is blended with acetone in an amount to make a volume ratio of acetone to water of 85:15-98:2, the NaCl content in the acetone-water solution containing the aimed compound is reduced, so that the aimed compound with a low Na content is obtained.
Inventors
- 👤 Hidetomo Ashitaka
- 👤 芦高 秀知
- 👤 Kazuya Jinda
- 👤 陣田 一也
- 👤 Yoshiyuki Miwa
- 👤 三輪 孔之
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