تفاعل #530779
ord-123f5fbc0e454a2988b953380176fc5f
معادلة التفاعل
1-phenyl-3-methyl-pyrazol-5-one
p-toluenesulphonic acid
acetic anhydride
→
1-phenyl-3-methyl-4-acetyl-pyrazol-5-one
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةare heated to the boil
- 2درجة الحرارةunder reflux for 6 hours
- 3workup.DISTILLATIONThe solvent is then distilled off under a water-pump vacuum
- 4workup.DISSOLUTIONthe residue is dissolved hot in 2 l of 5% strength sodium hydroxide solution
- 5أخرىis acidified with hydrochloric acid at room temperature
- 6ترشيحthe crystalline precipitate is filtered off
- 7غسيلwashed with water
- 8أخرىdried 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.