2-[2-(Azetidin-1-yl)-2-oxoethyl]-5-(benzyloxy)benzonitrile → 2-[2-(Azetidin-1-yl)-2-oxoethyl]-5-hydroxybenzonitrile

HRID 1850729ノート

反応式

HRID 1850729 の反応式
[N:1]1([C:5](=[O:23])[CH2:6][C:7]2[CH:14]=[CH:13][C:12]([O:15]CC3C=CC=CC=3)=[CH:11][C:8]=2[C:9]#[N:10])[CH2:4][CH2:3][CH2:2]1>C(O)C.[OH-].[OH-].[Pd+2]>[N:1]1([C:5](=[O:23])[CH2:6][C:7]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][C:8]=2[C:9]#[N:10])[CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 1

HCID 708186342-[2-(Azetidin-1-yl)-2-oxoethyl]-5-(benzyloxy)benzonitrile

生成物 1

HCID 708186242-[2-(Azetidin-1-yl)-2-oxoethyl]-5-hydroxybenzonitrile

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

2-[2-(azetidin-1-yl)-2-oxoethyl]-5-(benzyloxy)benzonitrile (410 mg, 1.34 mmol) was dissolved in ethanol (2 ml) and palladium hydroxide on carbon (20%) (94 mg, 0.134 mmol) added. The mixture was stirred under an atmosphere of hydrogen gas at RT overnight. The mixture was filtered and the filtrate concentrated under reduced pressure. The reside was purified by column chromatography using a Biotage RP C18 cartridge (30 g) using a gradient eluant of 0-25% water:acetonitrile+0.05% formic acid to afford the title compound. LC/MS (m/z): 217 (M+H)+.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customThe reside was purified by column chromatography

出典と根拠

ORDレコード
ord-744ba09762ec426fbcb8bd0e36c4bd50
出典データセット
uspto-grants-2015_02
特許番号
US08957062B2

反応ノート

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