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

HRID 1474681ノート

反応式

HRID 1474681 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

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-c1022e73178a46b38db8af53e381cf27
出典データセット
uspto-grants-2015_04
特許番号
US09018224B2

反応ノート

読み込み中…