반응 #63174

반응 방정식

ethyl p-aminobenzoylacetate

acetic anhydride

hydrazine hydrate

→

3-(4-acetylaminophenyl)-2-pyrazolin-5-one

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise to the solution at 40° C
2. 2
   온도After heat generation
3. 3
   workup.WAITthe reaction was further continued at a temperature between 55° C. and 60° C. for 1 hour
4. 4
   여과the precipitated crystals were filtered

실험 절차

In 440 ml of acetonitrile was dissolved 146 g of ethyl p-aminobenzoylacetate, and 70 ml of acetic anhydride was added dropwise to the solution at 40° C. After reacting at 40° C. for 1 hour, 48.8 g of 80% hydrazine hydrate was added thereto dropwise. After heat generation subsided, the reaction was further continued at a temperature between 55° C. and 60° C. for 1 hour. The reaction mixture was cooled to 5° C., and the precipitated crystals were filtered to yield 148 g of 3-(4-acetylaminophenyl)-2-pyrazolin-5-one as gray crystals having a melting point of 254° to 258° C.

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