These common heterocyclic compound, 110860-60-1, name is Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Product Details of 110860-60-1
(6) Synthesis of alpha-type crystal form azo pigment (1)-1 20.5 mL of acetic acid is cooled with ice to an internal temperature of 10C. 16.8 g of nitrosylfulfic acid is added with keeping the internal temperature at 15C or lower, and successively 9.5 g of the intermediate (b) is added thereto by portions with keeping the internal temperature at 15C or lower. After stirring for 15 minutes at an internal temperature of 15C, the internal temperature is increased to 25C in 15 minutes. After stirring for 90 minutes at the same temperature, 0.4 g of urea is added by portions at the same temperature, followed by stirring for 15 minutes at the same temperature to obtain a diazonium salt solution. Separately, 11.6 g of the intermediate (e) is completely dissolved in 405 mL of methanol at room temperature, and then the solution is cooled with ice to an internal temperature of -3C. At the same temperature, the above-described diazonium salt solution is added thereto by portions with keeping the internal temperature at 3C or lower and, after completion of the addition, the mixture is stirred for 2 hours to obtain an azo compound reaction solution. Separately, 810 mL of water is prepared, and the azo compound reaction solution is added thereto. The resulting mixture is stirred for 30 minutes at room temperature, and crystals precipitated are collected by filtration, spray-washed with 150 mL of methanol and, further, with 100 mL of water. The thus-obtained crystals are suspended in 750 mL of water without drying, and a 8-N potassium hydroxide aqueous solution is added thereto to adjust the pH to 5.7. After stirring for 20 minutes at room temperature, resulting crystals are collected by filtration, sufficiently spray-washed with water, and then spray-washed with 80 mL of methanol to obtain a crude pigment (1-1).
The synthetic route of Methyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.