Piperazine → 7-ethyl-2-piperazin-1-yl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

HRID 408097Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 408097
Cl[C:2]1[CH:3]=[N:4][C:5]2[CH2:11][CH2:10][N:9]([CH2:12][CH3:13])[CH2:8][CH2:7][C:6]=2[N:14]=1.[NH:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1>>[CH2:12]([N:9]1[CH2:10][CH2:11][C:5]2[N:4]=[CH:3][C:2]([N:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]3)=[N:14][C:6]=2[CH2:7][CH2:8]1)[CH3:13]

Komponenten

3

Edukt 2

HCID 4837PiperazineHCID 580715892-chloro-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

Produkt 1

HCID 580716007-ethyl-2-piperazin-1-yl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepineAusbeute 52,6 %

Reaktionsbedingungen

Temperatur
145 °C

Versuchsvorschrift

3 g 2-chloro-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine are combined with 23.3 g piperazine and the mixture is heated to 145° C. for 5 hours. Excess piperazine is distilled off and the residue is treated with dichloromethane and methanol. Any product precipitated is suction filtered and purified by chromatography (Alox, dioxane/toluene/methanol/NH4OH 50/20/20/2). 1.95 g product are obtained.

Aufarbeitung

  1. distillationExcess piperazine is distilled off
  2. additionthe residue is treated with dichloromethane and methanol
  3. customAny product precipitated
  4. filtrationfiltered
  5. custompurified by chromatography (Alox, dioxane/toluene/methanol/NH4OH 50/20/20/2)

Quellen und Nachweise

ORD-Eintrag
ord-beca2182d8fe4e4487d98701b8bf8b50
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08759326B2

Notizen zur Reaktion

Wird geladen…