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

HRID 622680노트

반응식

HRID 622680 반응식
[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

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 212915121-(2-Tetrahydrofurylmethyl)piperid-4-one oxime

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-09d6f6e35678469784fdaaf3b40fb39a
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772618

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