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Ethyl benzoylacetate → HCID 178433989, 화합물

HRID 1764094
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HRID 1764094 반응식
C(O[C:4](=[O:14])[CH2:5][C:6](=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)C.[NH2:15][C:16]1[N:20]([CH3:21])[N:19]=[C:18]([CH3:22])[CH:17]=1>O>[CH3:21][N:20]1[C:16]2=[N:15][C:6]([C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=3)=[CH:5][C:4]([OH:14])=[C:17]2[C:18]([CH3:22])=[N:19]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7170Ethyl benzoylacetateHCID 5207211,3-Dimethyl-1H-pyrazol-5-amine

생성물 1

HCID 178433989HCID 178433989, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

96 gms. of benzoylacetic acid ethyl ester (0.5 mol.) are added dropwise to a stirred mixture of 55.5 gms. of 5-amino-1,3-dimethylpyrazole (0.5 mol) and 250 gms. of polyphosphorus acid heated to 120° C. After the reaction has occurred, which can be recognized by the changing of the color, the whole is heated for an additional hour at 120° C. After the mixture has cooled to room temperature, 600 ml. of water are added and stirring is continued until the compound becomes crystalline. The mixture is allowed to stand overnight and is then filtered off. The collected 1,3-dimethyl-4-hydroxy-6-phenyl-1H-pyrazolo[3,4-b]pyridine is washed with dilute ammonia, dried and treated with ethyl acetate yielding 73.6 gms. (61.6%), m.p. 262°-264°.

후처리

  1. temperaturethe whole is heated for an additional hour at 120° C
  2. temperatureAfter the mixture has cooled to room temperature
  3. filtrationis then filtered off
  4. washThe collected 1,3-dimethyl-4-hydroxy-6-phenyl-1H-pyrazolo[3,4-b]pyridine is washed with dilute ammonia
  5. customdried
  6. additiontreated with ethyl acetate yielding 73.6 gms

출처 및 근거

ORD 기록
ord-7a008de488e842b6b3c7d19438a84541
출처 데이터셋
uspto-grants-1978_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04115394

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