Acetic Anhydride → 3-(4-Acetylaminophenyl)-2-pyrazolin-5-one

HRID 34896

반응식

HRID 34896 반응식
[NH2:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([CH2:8][C:9]([O:11]CC)=O)=O)=[CH:4][CH:3]=1.[C:16]([O:19]C(=O)C)(=O)[CH3:17].O.[NH2:24][NH2:25]>C(#N)C>[C:16]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]2[CH2:8][C:9](=[O:11])[NH:25][N:24]=2)=[CH:14][CH:15]=1)(=[O:19])[CH3:17]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 24654Hydrazine hydrate (1:1)HCID 3045879Acetic acid, (p-aminobenzoyl)-, ethyl ester (6CI,7CI)

생성물 1

HCID 138791443-(4-Acetylaminophenyl)-2-pyrazolin-5-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
5 °C

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.

후처리

  1. additionwas added dropwise to the solution at 40° C
  2. temperatureAfter heat generation
  3. waitthe reaction was further continued at a temperature between 55° C. and 60° C. for 1 hour
  4. filtrationthe precipitated crystals were filtered

출처 및 근거

ORD 기록
ord-08d6d7f94b4f4cc897e7e0b7b69e8795
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764458

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