تفاعل #530779

ord-123f5fbc0e454a2988b953380176fc5f

معادلة التفاعل

Cc1cc(=O)n(-c2ccccc2)[nH]1
1-phenyl-3-methyl-pyrazol-5-one
Cc1ccc(S(=O)(=O)O)cc1
p-toluenesulphonic acid
CC(=O)OC(C)=O
acetic anhydride
CC(=O)c1c(C)[nH]n(-c2ccccc2)c1=O
1-phenyl-3-methyl-4-acetyl-pyrazol-5-one

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةare heated to the boil
  2. 2
    درجة الحرارةunder reflux for 6 hours
  3. 3
    workup.DISTILLATIONThe solvent is then distilled off under a water-pump vacuum
  4. 4
    workup.DISSOLUTIONthe residue is dissolved hot in 2 l of 5% strength sodium hydroxide solution
  5. 5
    أخرىis acidified with hydrochloric acid at room temperature
  6. 6
    ترشيحthe crystalline precipitate is filtered off
  7. 7
    غسيلwashed with water
  8. 8
    أخرىdried in vacuo at 40° C

الإجراء التجريبي

174 g of 1-phenyl-3-methyl-pyrazol-5-one in 700 ml of acetic anhydride, with the addition of 6 g of p-toluenesulphonic acid, are heated to the boil under reflux for 6 hours. The solvent is then distilled off under a water-pump vacuum, the residue is dissolved hot in 2 l of 5% strength sodium hydroxide solution, the solution is clarified with 8 g of active charcoal, the filtrate is acidified with hydrochloric acid at room temperature and the crystalline precipitate is filtered off, washed with water and dried in vacuo at 40° C. 183 g of 1-phenyl-3-methyl-4-acetyl-pyrazol-5-one are obtained in the form of colourless crystal needles.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04260776uspto-grants-1981_04