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Ammonium Chloride → HCID 66941861, Verbindung

HRID 2267224
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2267224
C[Mg]Cl.[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)([C:17]#N)[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[NH4+].[Cl-]>C1COCC1>[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]2)([CH3:17])[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 20117869HCID 20117869, VerbindungHCID 178418332HCID 178418332, Verbindung

Produkt 1

HCID 66941861HCID 66941861, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

15 mL methylmagnesium chloride solution (45 mmol, 3 M in THF) were added at RT to 2.37 g (7.92 mmol) 1-benzyl-4-piperazin-1-yl-piperidine-4-carbonitrile in 100 mL dry THF and the reaction mixture was stirred for 3 h. Saturated NH4Cl solution was added, the mixture was stirred for another 10 min, the aqueous phase was washed with EtOAc, combined with 4 M NaOH solution until an alkaline reaction was obtained, extracted exhaustively with DCM and the combined organic phases were dried over Na2SO4. After elimination of the desiccant and solvent the residue was further reacted without any further purification.

Aufarbeitung

  1. stirringthe mixture was stirred for another 10 min
  2. washthe aqueous phase was washed with EtOAc
  3. customcombined with 4 M NaOH solution until an alkaline reaction
  4. customwas obtained
  5. extractionextracted exhaustively with DCM
  6. dry with materialthe combined organic phases were dried over Na2SO4
  7. customAfter elimination of the desiccant and solvent the residue was further reacted without any further purification

Quellen und Nachweise

ORD-Eintrag
ord-7de95d38cf6c48f781a1718a104cb955
Quelldatensatz
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07858622B2

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