반응 #816372

반응 방정식

4-amino-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one

meta-phenylene diamine

ammonium persulfate

ammonia

→

expected product

수율 30.0%

4-{[(1E)-2-amino-4-iminocyclohexa-2,5-dien-1-ylidene]amino}-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one

수율 30.0%

용매

—

ice water

water

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred at 0° C. for 1 h 30 min
2. 2
   기타the solid formed
3. 3
   기타was separated by filtration
4. 4
   세척washed with water and acetone
5. 5
   기타dried in a desiccator under vacuum for 12 hours

실험 절차

20 mmol of 4-amino-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one and 20 mmol of meta-phenylene diamine was dissolved in 30 g of an ice/water mixture and the pH was adjusted to 10 using 20 ml of 20% aqueous ammonia. While stirring, a solution of 24 mmol of ammonium persulfate in 10 ml of water was added dropwise over 30 minutes. The mixture was stirred at 0° C. for 1 h 30 min and the solid formed was separated by filtration and washed with water and acetone and dried in a desiccator under vacuum for 12 hours, which resulted in 1.8 g of expected product, or a yield of 30%.

출처