반응 #155900

반응 방정식

1-phenylhydrazine

2-(1-ethoxyethylidene)malononitrile

ethoxymethylene malononitrile

→

5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile

용매

ethanol

반응 조건

후처리

1. 1
   기타Into a 250-mL 3-necked round-bottom flask, was placed
2. 2
   기타at room temperature
3. 3
   기타at room temperature
4. 4
   workup.ADDITIONAfter about half of the addition
5. 5
   온도the solution was carefully heated to boiling
6. 6
   온도the resulting solution was heated
7. 7
   온도to reflux for 4 hr
8. 8
   온도The resulting mixture was then cooled with a water/ice bath
9. 9
   여과the solids were collected by filtration

실험 절차

Into a 250-mL 3-necked round-bottom flask, was placed a solution of 1-phenylhydrazine (31.5 g, 291.67 mmol, 1.14 equiv) in ethanol (105 mL) at room temperature. To the resulting mixture was then added 2-(1-ethoxyethylidene)malononitrile (35 g, 257.35 mmol, 1.00 equiv) in several batches at room temperature. After about half of the addition was completed, the solution was carefully heated to boiling. After all the ethoxymethylene malononitrile was added, the resulting solution was heated to reflux for 4 hr. The resulting mixture was then cooled with a water/ice bath, and the solids were collected by filtration to yield 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile as a yellow solid.

출처