Water → Quinolizidin-2-ylmethylamine

HRID 609620노트

반응식

HRID 609620 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([CH:9]1[CH2:18][CH2:17][N:16]2[CH:11]([CH2:12][CH2:13][CH2:14][CH2:15]2)[CH2:10]1)#[N:8].O.[OH-].[Na+]>C1COCC1>[CH2:10]1[CH:11]2[N:16]([CH2:15][CH2:14][CH2:13][CH2:12]2)[CH2:17][CH2:18][CH:9]1[CH2:7][NH2:8]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 125773752-CyanoquinolizidineHCID 21226445Aluminium lithium hydride

생성물 1

HCID 82413010Quinolizidin-2-ylmethylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A stirred suspension of lithium aluminium hydride (400 mg, 0.010 mole) in THF (20 ml) at room temperature under nitrogen was treated with a solution of eq-2-cyanoquinolizidine (E. Koshinaka et al, Yakugaku Zasshi 1980, 100, 88) in THF (3 ml) and the mixture then heated under reflux for 20 minutes. The mixture was allowed to cool then treated cautiously with water (0.4 ml), 10% NaOH solution (0.4 ml) and water (1.2 ml). The resulting mixture was filtered and the filtrate concentrated in vacuo. The residue was distilled in a Kugelrohr apparatus to afford the title compound (D13); as a colourless oil (700 mg, 97%).

후처리

  1. temperaturethe mixture then heated
  2. temperatureunder reflux for 20 minutes
  3. temperatureto cool
  4. filtrationThe resulting mixture was filtered
  5. concentrationthe filtrate concentrated in vacuo
  6. distillationThe residue was distilled in a Kugelrohr apparatus

출처 및 근거

ORD 기록
ord-9bb4aaffe7ff4be9a9340781449ff40b
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998409

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