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Tetrahydrofuran → HCID 90991820, 화합물

HRID 1800574
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HRID 1800574 반응식
[C:1]([O:5][C:6](=[O:25])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[C:10]([O:15][C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][N:17]=2)[CH:9]=1)([CH3:4])([CH3:3])[CH3:2].O1CCCC1>CO.[C].[Pd]>[C:1]([O:5][C:6](=[O:25])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[C:10]([O:15][C:16]2[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][N:17]=2)[CH:9]=1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8028TetrahydrofuranHCID 91362017HCID 91362017, 화합물

생성물 1

HCID 90991820HCID 90991820, 화합물수율 73.2%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

A suspension of tert-butyl{4-fluoro-3-[(5-nitropyridin-2-yl)oxy]phenyl}carbamate (3.75 g, 10.7 mmol) and 10% palladium-carbon (0.5 g) in methanol (10 mL)-tetrahydrofuran (10 mL) was vigorously stirred at room temperature under a hydrogen atmosphere overnight. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was poured into water (100 mL), and the mixture was extracted with ethyl acetate (100 mL×2). The ethyl acetate layers were combined and dried over anhydrous sodium sulfate, and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure, and the residue was triturated with diethyl ether to give the title compound (2.50 g, 73%) as a pale-yellow amorphous.

후처리

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionThe residue was poured into water (100 mL)
  4. extractionthe mixture was extracted with ethyl acetate (100 mL×2)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationthe insoluble material was filtered off
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe residue was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-3231c59aa05b41918aeba374f63bc14e
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08344135B2

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