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Ammonium Chloride → HCID 22502565, Verbindung

HRID 1251177
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1251177
[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[C:14]3[CH:15]=[CH:16][S:17][C:13]=3[CH:12]=[C:11]([C:18]3[CH:23]=[CH:22][C:21]([CH:24]=[O:25])=[CH:20][CH:19]=3)[N:10]=2)[CH2:5][CH2:4]1)[CH3:2].[CH2:26]([Mg]Br)[CH3:27].C(OCC)C.[Cl-].[NH4+]>O1CCCC1>[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[C:14]3[CH:15]=[CH:16][S:17][C:13]=3[CH:12]=[C:11]([C:18]3[CH:23]=[CH:22][C:21]([CH:24]([OH:25])[CH2:26][CH3:27])=[CH:20][CH:19]=3)[N:10]=2)[CH2:5][CH2:4]1)[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 22502581HCID 22502581, VerbindungHCID 178467792HCID 178467792, Verbindung

Produkt 1

HCID 22502565HCID 22502565, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 4-(4-ethylpiperazin-1-yl)-6-(4-formylphenyl)thieno[3,2-c]pyridine (0.20 g) in tetrahydrofuran (20 ml) was added 3M ethylmagnesium bromide/diethyl ether solution (0.5 ml), and the mixture was reacted at room temperature for 30 min. To the resulting reaction solution was added an aqueous solution of ammonium chloride, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried. The resulting product was filtered through NH silica gel and washed with ethyl acetate. The filtrate was concentrated, to give 0.17 g of the title compound as white crystals.

Aufarbeitung

  1. customthe mixture was reacted at room temperature for 30 min
  2. customTo the resulting reaction solution
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and brine
  5. customdried
  6. filtrationThe resulting product was filtered through NH silica gel
  7. washwashed with ethyl acetate
  8. concentrationThe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-b8b576171af04f51a8aca26bedf2d2c2
Quelldatensatz
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06340759B1

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