5-CHLORO-1,3-DIMETHYL-1H-PYRAZOLE-4-CARBONITRILE synthesis
- Product Name:5-CHLORO-1,3-DIMETHYL-1H-PYRAZOLE-4-CARBONITRILE
- CAS Number:96286-02-1
- Molecular formula:C6H6ClN3
- Molecular Weight:155.58
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Yield:96286-02-1 90%
Reaction Conditions:
with ammonium hydroxide;sodium bromate;acetic acid in water at 90 - 100; for 1 h;
Steps:
5 Synthesis of 1,3-dimethyl-5-chloro-1H-pyrazole-4-carbonitrile
in room temperature, Mixing 1,3-dimethyl-5-chloro-1H-pyrazole-4-carbaldehyde (15.9 g, 0.1 mol), sodium bromate (45.3 g, 0.3 mol) and 100 g of acetic acid, adding 25 g of ammonia Ammonia water with a molecular mass concentration of 25% and 1000 ml of water are heated to 90 °C, the reaction is exothermic, the reaction temperature is maintained at 100 ° C, and the reaction is refluxed for 1 hour. 1,3-Dimethyl-5-chloro-1H-pyrazole-4-carbaldehyde is completely reacted and cooled to room temperature.The reaction solution was poured into ice water to quench and dilute, neutralized until the reaction solution was neutral, extracted with dichloromethane, dried, concentrated, and distilled under reduced pressure and recrystallized.The product was obtained in 14 g, the yield was 90%, and the purity was over 99%.
References:
CN108707113,2018,A Location in patent:Paragraph 0025
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