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Tetrahydrofuran → HCID 90991820、化合物

HRID 1800574
ノート
印刷プレビュー

反応式

HRID 1800574 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8028TetrahydrofuranHCID 91362017HCID 91362017、化合物

生成物 1

HCID 90991820HCID 90991820、化合物収率 73.2%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3231c59aa05b41918aeba374f63bc14e
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08344135B2

反応ノート

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