HCID 18318541, 화합물 → 1-Methylpyrrolidine-3-ethanol

HRID 2259711노트

반응식

HRID 2259711 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH:7][CH2:8][CH2:9][CH:10]1[CH2:14][CH2:13][N:12]([CH3:15])[C:11]1=O>>[CH3:15][N:12]1[CH2:13][CH2:14][CH:10]([CH2:9][CH2:8][OH:7])[CH2:11]1

참가 물질

3

반응물 2

HCID 18318541HCID 18318541, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 211911231-Methylpyrrolidine-3-ethanol수율 52.9%

실험 절차

Lithium aluminium hydride (347 mg) was cautiously added, in portions, to a vigorously stirred suspension of 3-(2-hydroxyethyl)-1-methyl-2-pyrrolidinone (886 mg) in dry, freshly distilled tetrahydrofuran (60 ml), at 5° under nitrogen. The resultant suspension was stirred and heated at reflux under nitrogen for 1 h. The mixture was cooled to 5°, with stirring, and cautiously treated with a mixture of water (1 ml) and tetrahydrofuran (10 ml). The solvents were evaporated, the residue dissolved in ethanol and the solvent was again removed, in vacuo. The residue was chromatographed using dichloromethane:ethanol:ammonia (25.8:1) as eluent, to give the title compound (423 mg).

후처리

  1. customin dry
  2. customat 5°
  3. temperatureheated
  4. temperatureat reflux under nitrogen for 1 h
  5. temperatureThe mixture was cooled to 5°
  6. stirringwith stirring
  7. additioncautiously treated with a mixture of water (1 ml) and tetrahydrofuran (10 ml)
  8. customThe solvents were evaporated
  9. dissolutionthe residue dissolved in ethanol
  10. customthe solvent was again removed, in vacuo
  11. customThe residue was chromatographed

출처 및 근거

ORD 기록
ord-193a23b0d3e44245abee774810cb5e87
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05475020

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