Sodium Hydroxide → Chromium(III) 3,5-di-tert-butylsalicylate

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반응 단계

450 g of water and 7.2 g of NaOH were placed in a 500-cc beaker, and the mixture was heated under stirring to completely dissolve NaOH. This NaOH aqueous solution was heated to 65° C., and 45 g of 3,5-di-tert-butylsalicylic acid was added thereto under stirring. The mixture was further stirred while keeping the temperature at 65° C. to dissolve 3,5-di-tert-butylsalicylic acid. When pH of the dissolved solution became 6.8, heating and stirring were discontinued, and the solution was filtered to remove insoluble 3,5-di-tert-butylsalicylic acid, thus a brown filtrate being obtained. Separately, 37.2 g of a 40% CrCl3 solution and 120 g of water were placed in a 500-cc beaker to prepare a chromium(III) chloride solution having a pH of 2.1. To this chromium(III) chloride solution was gradually added 120 g of 1% NaOH aqueous solution with spending enough time to obtain a solution of 3.95 in pH. Then, this solution was transferred into a 2-liter beaker, and diluted with water to make the total amount 350 g. This chromium(III) chloride solution was heated to 60° C. and, under stirring, the above-described solution of 3,5-di-tert-butylsalicylic acid kept at 60° C. was dropwise added thereto over a period of time of 1.5 to 2 hours. As the addition proceeded, the reaction solution gradually assumed a light green color. After completion of the dropwise addition, stirring was further continued for 1 hour at a temperature of 60 to 65° C., and the reaction solution was suction filtered and washed with water to obtain 170 g of a reaction product (wet). The pH of the filtrate was 4.00. The reaction product collected by filtration was dried at 50° C. for about 14 hours, and the dried product was pulverized to obtain 70 g of an end product. The reaction product is completely soluble in carbon tetrachloride.

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