HCID 18318541、化合物 → 1-Methylpyrrolidine-3-ethanol

HRID 2259711ノート

反応式

HRID 2259711 の反応式
[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

参加物

3

反応物 2

HCID 18318541HCID 18318541、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 211911231-Methylpyrrolidine-3-ethanol収率 52.9%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-193a23b0d3e44245abee774810cb5e87
出典データセット
uspto-grants-1995_12
特許番号
US05475020

反応ノート

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