反应详情

温度

70 °C

Method B Polyphosphoric acid (500 g) was added to a 1 L flask equipped with an overhead stirrer and heated to 70° C. under nitrogen. A blended mixture of 4-nitro-3-pyrazole carboxylic acid (50 g) and 1,2-diamino-4,5-dimethylbenzene (43.4 g) was added and the mixture was heated to 180° C. After 1 hour at this temperature the reaction mixture was cooled to 130° C. and poured into ice water (2.5 kg). This mixture was stirred with an overhead stirrer and then treated with aqueous ammonium hydroxide (350 mL, 30%) until the pH was 2.1. After stirring for a further 15 minutes the mixture was filtered and the filtered solid was washed three times with water (200 mL) then dried under vacuum to give 4-nitro-1H-pyrazole-3-carboxylic acid (2-amino-4,5-dimethylphenyl)amide as a brown solid.

1. customequipped with an overhead stirrer
2. additionwas added
3. temperaturethe mixture was heated to 180° C
4. temperatureAfter 1 hour at this temperature the reaction mixture was cooled to 130° C.
5. stirringAfter stirring for a further 15 minutes the mixture
6. filtrationwas filtered
7. washthe filtered solid was washed three times with water (200 mL)
8. customthen dried under vacuum