2-methyl-5-chloro-1,4-diaminobenzene and its prepn and application
A technology of p-phenylenediamine and methyl, applied in the field of 2-methyl-5-chloro-1, can solve problems such as no synthesis method, and achieve the effects of wide application, high output value and mild reaction conditions
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[0010] Add 14.2g of 2-methyl-5-chloro-aniline, 120mL of 60% acetic acid, and 16.5mL of acetic anhydride into a 250mL three-necked flask, stir and react at 70-75°C for 1.5h, pour 5 times the amount of ice containing 10% NaCl Disperse in aqueous solution, filter, and dry to obtain white product N-acetyl-2-methyl-5-chloro-aniline, about 18.2 g, yield 99%, melting point 135-136°C.
[0011] Put 14.7g of the above self-made N-acetyl-2-methyl-5-chloro-aniline into a 250mL three-necked flask, add 45mL of glacial acetic acid and 58mL of concentrated sulfuric acid, heat to 40°C, stir to dissolve, cool to room temperature, and slowly drop Add 21 mL of nitric acid, stir and react at room temperature for 2 hours, pour into 5 times the amount of ice water to disperse, filter, wash the product with water until pH = 5, and dry to obtain the light yellow product N-acetyl-2-methyl-4-nitro-5 -Chloro-aniline 17.3g, yield about 95%.
[0012] Put 11.4 g of the above nitrated product in a 250 mL th...
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