p-ter-ブチールフェノールのニトロ化に就いて

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In this paper the authors have studied the mononitration of p-ter-butylphenol to obtain p-ter-butyl-o-nitrophenol, which is a starting material of p-ter-butyl-o-anisidine, intermediate of azodyes. The procedure is as follws; 30g of p-ter-butylphenol is added, by the portion of 0.5-1g, to a solution of 18.3g water, 22.6g nitric acid (sp. gr. 1.38) and 8g sulphuric acid (sp. gr. 1.84), in a 300c. c. three necked flask, for 20 minutes, under rapid stirring and good cooling. The temperature is kept at 15-18℃. through the addition. Further, the mixture is stirred at 10-15℃. for 1.5 Hours to complete the reaction. At the end, the mixture is poured into 80g ice and 50g water, and the precipitated product is filtered under cooling. To remove adhering acid, the crude product is washed thoroughly with 50c.c. water many times, and then it distilled with steam for the purification. A pale yellow oil in water distillate of about 1500c.c. thus obtained, is cooled at 0℃ to crystallise the p-ter-butyl-o-nitrophenol. The crystalline product is filtered and dried over sulphuric acid in vacuum desicator. The yield of product (m. p. 25.5℃) is 32.5g (83.5%). The above product is recrystallised from methanol for the complete purification, the result being a pale yellow thin plate Crystal of m. p. 26℃ (this differs from m. p. 95℃. in a literature : Carlgelzer, B.21, 2947). K-, Na- and Ba-salts are yellow but characterised by the colour change from yellow to vermillion red under heating in solution or solid state.
山形大学の論文
1954-05-28

p-ter-ブチールフェノールのニトロ化に就いて

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