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Formamidine acetate → tert-butyl 4-(4-oxo-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-7-yl)piperidine-1-carboxylate

HRID 1616087
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HRID 1616087 반응식
[NH2:1][C:2]1[C:3]([CH:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)=[CH:4][NH:5][C:6]=1[C:7]([O:9]CC)=O.C(O)(=O)C.[CH:29](N)=[NH:30]>C(O)C>[O:9]=[C:7]1[NH:30][CH:29]=[N:1][C:2]2[C:3]([CH:12]3[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:23])([CH3:24])[CH3:22])=[O:19])[CH2:14][CH2:13]3)=[CH:4][NH:5][C:6]1=2
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참가 물질

4

반응물 2

HCID 160693Formamidine acetateHCID 86681878tert-butyl 4-[4-amino-5-(ethoxycarbonyl)-1H-pyrrol-3-yl]piperidine-1-carboxylate

생성물 1

HCID 136359803tert-butyl 4-(4-oxo-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-7-yl)piperidine-1-carboxylate수율 102.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

tert-Butyl 4-[4-amino-5-(ethoxycarbonyl)-1H-pyrrol-3-yl]piperidine-1-carboxylate (466 mg, 1.38 mmol) was dissolved in ethanol (8 mL), and then formamidine acetate (863 mg, 8.29 mmol) was added, followed by heating under reflux for 14 hours. The reaction liquid was cooled, and the precipitated solid was filtered and washed with ethanol to give tert-butyl 4-(4-oxo-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-7-yl)piperidine-1-carboxylate (452 mg, >1000) as a pale yellow solid.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 14 hours
  3. customThe reaction liquid
  4. temperaturewas cooled
  5. filtrationthe precipitated solid was filtered
  6. washwashed with ethanol

출처 및 근거

ORD 기록
ord-faf481bf407044ebba0534fb8efb0f40
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765771B2

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