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Acetic Acid → 4-{[(2S)-2-fluoropropyl]oxy}piperidine

HRID 69126
ノート
印刷プレビュー

反応式

HRID 69126 の反応式
[F:1][C@@H:2]([CH3:11])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1.C(O)(=O)C>CO.[Pd]>[F:1][C@@H:2]([CH3:11])[CH2:3][O:4][CH:5]1[CH2:6][CH2:7][NH:8][CH2:9][CH2:10]1
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 176Acetic AcidHCID 666961134-{[(2S)-2-fluoropropyl]oxy}pyridine

生成物 1

HCID 866943284-{[(2S)-2-fluoropropyl]oxy}piperidine収率 43.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

2.2 g of 4-{[(2S)-2-fluoropropyl]oxy}pyridine was added to a solution of 22 mL of acetic acid in 22 mL of methanol, and 500 mg of 10% palladium on carbon (wet type) was added thereto under an argon atmosphere. The mixture was stirred at room temperature overnight under a hydrogen atmosphere of 3 atm. The reaction mixture was filtered through celite and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (chloroform/methanol) to obtain 988 mg of 4-{[(2S)-2-fluoropropyl]oxy}piperidine.

後処理

  1. additionwas added
  2. filtrationThe reaction mixture was filtered through celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by basic silica gel column chromatography (chloroform/methanol)

出典と根拠

ORDレコード
ord-5bcb731dbce54b409b27b111188b01a7
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822448B2

反応ノート

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