4-Pyridineacetic acid hydrochloride → 4-Piperidineacetic acid

HRID 29748

反応式

HRID 29748 の反応式
Cl.[N:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1>O>[NH:2]1[CH2:7][CH2:6][CH:5]([CH2:8][C:9]([OH:11])=[O:10])[CH2:4][CH2:3]1

参加物

3

実験手順

Pyridin-4-yl-acetic acid hydrochloride (20.0 g, 115 mmol) was added to water/25% ammonia (125 mL:10 mL). The mixture was degassed and flushed with nitrogen before addition of rhodium on activated alumina (0.45 g). The mixture was again degassed, then stirred in a hydrogen atmosphere at 50 bar for 16 h. Filtration of the reaction mixture through filter paper afforded the bulk of the catalyst which was recycled after washing with methanol. The filtrate was then filtered through Celite and concentrated to afford a white solid (19.7 g, 96% yield).

後処理

  1. customThe mixture was degassed
  2. customflushed with nitrogen before addition of rhodium on activated alumina (0.45 g)
  3. customThe mixture was again degassed
  4. filtrationFiltration of the reaction mixture
  5. filtrationthrough filter paper
  6. customafforded the bulk of the catalyst which
  7. washafter washing with methanol
  8. filtrationThe filtrate was then filtered through Celite
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-6d36eb0a15c64286b6d786d4f3d46abd
出典データセット
uspto-grants-2008_09
特許番号
US07423012B2

関連ノート

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