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Ethyl Acetoacetate → 2-Indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one

HRID 384289
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인쇄 미리보기

반응식

HRID 384289 반응식
[CH2:1]1[C:9]2[C:4](=[CH:5][C:6]([NH:10][NH2:11])=[CH:7][CH:8]=2)[CH2:3][CH2:2]1.[C:12](OCC)(=[O:17])[CH2:13][C:14]([CH3:16])=O>C(O)(=O)C>[CH2:1]1[C:9]2[C:4](=[CH:5][C:6]([N:10]3[C:12](=[O:17])[CH2:13][C:14]([CH3:16])=[N:11]3)=[CH:7][CH:8]=2)[CH2:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 8868Ethyl AcetoacetateHCID 217018272,3-Dihydro-1H-inden-5-ylhydrazine

생성물 1

HCID 574837802-Indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one수율 62.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

Indan-5-yl-hydrazine 1h (2.05 g, 13.8 mmol) was dissolved in 50 mL of acetic acid followed by addition of ethyl acetoacetate (1.76 mL, 13.8 mmol). The reaction mixture was heated at 100° C. overnight and the reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel column chromatography to obtain the title compound 2-indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one 1i (1.84 g, yield 62.3%) as a yellow solid.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-9e018d116e9341f7801e9463fc0d14f8
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367710B2

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