Water → 1-[(Oxolan-2-yl)methyl]piperidin-4-amine

HRID 622680ノート

反応式

HRID 622680 の反応式
[O:1]1[CH2:5][CH2:4][CH2:3][CH:2]1[CH2:6][N:7]1[CH2:12][CH2:11][C:10](=[N:13]O)[CH2:9][CH2:8]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[O:1]1[CH2:5][CH2:4][CH2:3][CH:2]1[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([NH2:13])[CH2:11][CH2:12]1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 212915121-(2-Tetrahydrofurylmethyl)piperid-4-one oxime

生成物 1

HCID 167746731-[(Oxolan-2-yl)methyl]piperidin-4-amine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1-(2-tetrahydrofurylmethyl)piperid-4-one oxime (42.5 g; 0.22 moles) in anhydrous tetrahydrofuran (700 ml) was added dropwise to a suspension of lithium aluminium hydride (24.4 g; 0.64 moles) in anhydrous tetrahydrofuran (300 ml). The reaction mixture was left with stirring at room temperature overnight and then, water (24.5 ml), 4N sodium hydroxide aqueous solution (24.5 ml) and water (73.5 ml) were successively added, filtered, the filtrates dried (Na2SO4) and brought to dryness in vacuo. The resulting oil (28 g) was distilled to give 1-(2-tetrahydrofurylmethyl)-4-aminopiperidine, boiling point 94°-98° C./0.2 mm Hg.

後処理

  1. waitThe reaction mixture was left
  2. filtrationfiltered
  3. dry with materialthe filtrates dried (Na2SO4)
  4. distillationThe resulting oil (28 g) was distilled

出典と根拠

ORDレコード
ord-09d6f6e35678469784fdaaf3b40fb39a
出典データセット
uspto-grants-1988_09
特許番号
US04772618

反応ノート

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