Water → HCID 21409899, Verbindung

HRID 1283543Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1283543
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([NH:10][CH2:11][C:12]1([N:18]2[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)(=O)[CH3:8].O>O1CCCC1>[CH2:7]([NH:10][CH2:11][C:12]1([N:18]2[CH2:19][CH2:20][N:21]([CH3:24])[CH2:22][CH2:23]2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)[CH3:8]

Komponenten

5

Edukt 3

HCID 962WaterHCID 21226445Aluminium lithium hydride2×HCID 21409820HCID 21409820, Verbindung

Produkt 1

HCID 21409899HCID 21409899, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a stirred solution of lithium aluminium hydride (3 g.,) in dry tetrahydrofuran (40 ml) was added a solution of 1-[1-(Acetamidomethyl)cyclohexyl]-4-methyl piperazine (3 g.,) in dry tetrahydrofuran (40 ml) dropwise. The stirring was continued overnight, the suspension was heated under reflux for a further 6 hrs. and the excess LiAlH4 neutralised with water. The mixture was filtered and the filtrate was dried (anhyd. Na2SO4) and evaporated to an oil, which was micro distilled to give 1-[1-(Ethylaminomethyl)cyclohexyl]-4-methyl piperazine as a colourless oil. b.p. 35mm 105°-109° (1.96 g., 69%)

Aufarbeitung

  1. temperaturethe suspension was heated
  2. temperatureunder reflux for a further 6 hrs
  3. filtrationThe mixture was filtered
  4. dry with materialthe filtrate was dried (anhyd. Na2SO4)
  5. customevaporated to an oil, which
  6. distillationwas micro distilled

Quellen und Nachweise

ORD-Eintrag
ord-e4aef959692f45f49a4bf64827e2aabf
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03975443

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