Water → 2-(4-Phenylpiperazin-1-yl)ethan-1-amine

HRID 1439600Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1439600
[C:1]([CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)#[N:2].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[Na+]>O1CCCC1>[NH2:2][CH2:1][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5]1

Komponenten

6

Edukt 4

HCID 962Water2×HCID 14798Sodium HydroxideHCID 4372382-(4-Phenylpiperazin-1-yl)acetonitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 47425032-(4-Phenylpiperazin-1-yl)ethan-1-amineAusbeute 76,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 600 g 1-Cyanomethyl-4-phenylpiperazine in 1525 ml tetrahydrofuran was added dropwise to a suspension of 181 g LiAlH4 in 4.5 liters tetrahydrofuran. The mixture was refluxed 18 hours, cooled and added 181 ml water, 181 ml 15% NaOH, and 543 ml water. The mixture was filtered and concentrated to dryness on the rotovap and the residue distilled to give 470 g product, b0.1 117-24°, m.50-7°.

Aufarbeitung

  1. temperatureThe mixture was refluxed 18 hours
  2. temperaturecooled
  3. filtrationThe mixture was filtered
  4. concentrationconcentrated to dryness on the rotovap
  5. distillationthe residue distilled

Quellen und Nachweise

ORD-Eintrag
ord-005dd94f01924cd58f2d786a207ecf3b
Quelldatensatz
uspto-grants-1977_11
Patentnummer
US04060526

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