تفاعل #816372

ord-8179a22236034f70bf4460853eb432f8

معادلة التفاعل

Cc1c(N)c(=O)n(-c2ccccc2)n1C
4-amino-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one
Nc1cccc(N)c1
meta-phenylene diamine
O=S(=O)([O-])OOS(=O)(=O)[O-].[NH4+].[NH4+]
ammonium persulfate
N
ammonia
Cc1c(/N=C2\C=CC(=N)C=C2N)c(=O)n(-c2ccccc2)n1C
expected product
المردود 30.0%
Cc1c(/N=C2\C=CC(=N)C=C2N)c(=O)n(-c2ccccc2)n1C
4-{[(1E)-2-amino-4-iminocyclohexa-2,5-dien-1-ylidene]amino}-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one
المردود 30.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07582123B2uspto-grants-2009_09