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Ethyl 2-(3-formylphenoxy)acetate → HCID 178472964, 화합물

HRID 1597858
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인쇄 미리보기

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HRID 1597858 반응식
[CH:1]1([N:6]2[C:10]([NH2:11])=[C:9]([C:12]([NH2:14])=[O:13])[C:8]([CH2:15][CH3:16])=[N:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:17]([O:19][C:20]([CH2:22][O:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][CH:31]=1)[CH:27]=O)=[O:21])[CH3:18]>>[CH:1]1([N:6]2[C:10]3=[N:11][C:27]([C:26]4[CH:29]=[CH:30][CH:31]=[C:24]([O:23][CH2:22][C:20]([O:19][CH2:17][CH3:18])=[O:21])[CH:25]=4)=[N:14][C:12](=[O:13])[C:9]3=[C:8]([CH2:15][CH3:16])[NH:7]2)[CH2:2][CH2:3][CH2:4][CH2:5]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 1494377Ethyl 2-(3-formylphenoxy)acetateHCID 224493525-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide

생성물 1

HCID 178472964HCID 178472964, 화합물수율 37.9%

반응 조건

온도
160 °C

실험 절차

A mixture of 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (3.54 g, 15.95 mmol), 3-(ethoxycarbonylmethoxy) benzaldehyde (4.3 g) and xylenes (20 ml) was heated at 160° C. overnight. The reaction mixture was cooled to room temperature, a solid formed which was collected by filtration and washed with methanol and then ether. The product was recrystallized from acetonitrile to afford 2.48 g of 1-cyclopentyl-3-ethyl-6-[3-(ethoxycarbonylmethoxy)phenyl]pyrazolo[3,4-d]pyrimidin-4-one. An additional 0.3 g of product was also obtained from the recrystallization of the filtrate for a total of 2.78 g.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customa solid formed which
  3. filtrationwas collected by filtration
  4. washwashed with methanol
  5. customThe product was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-a6c8c7c76d2142eca150bb11780362e4
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05736548

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