4-Pyridineacetic acid hydrochloride → 4-Piperidineacetic acid

HRID 29748

반응식

HRID 29748 반응식
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

참가 물질

3

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6d36eb0a15c64286b6d786d4f3d46abd
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423012B2

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