Thionyl Chloride → HCID 22024658, Verbindung

HRID 501008Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 501008
[Br:1][C:2]1[C:3]([NH:8][CH:9]([CH2:12][CH3:13])[CH2:10]O)=[N:4][CH:5]=[N:6][CH:7]=1.S(Cl)(Cl)=O>C1(C)C(C)=CC=CC=1>[Br:1][C:2]1[C:3]2[N:4]([CH2:10][CH:9]([CH2:12][CH3:13])[N:8]=2)[CH:5]=[N:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 22024679HCID 22024679, Verbindung

Produkt 1

HCID 22024658HCID 22024658, VerbindungAusbeute 98,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2-[(5-Bromo-4-pyrimidinyl)amino]-1-butanol (3.3 g) was dissolved in xylene (27 mL), then thionyl chloride (4.9 mL) was added thereto, and the mixture was heated under stirring at 100° C. for 1 day. The precipitated crystals were collected by filtration and suspended in a 1M aqueous sodium carbonate solution. This mixture was extracted with dichloromethane to give the crude title compound (3.0 g) as an orange oil. This title compound was used in the next reaction without purification.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. filtrationThe precipitated crystals were collected by filtration
  3. extractionThis mixture was extracted with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-281fe9257f52469ab646f0b24a9f47fc
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772249B2

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