Thionyl Chloride → HCID 178499150, Verbindung

HRID 1971071Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1971071
[CH2:1]([N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[C:18]([O:20][CH3:21])=[O:19])[CH2:9][CH2:10]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:24])=O>C(Cl)Cl>[ClH:24].[CH2:1]([N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[C:18]([O:20][CH3:21])=[O:19])[CH2:9][CH2:10][Cl:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 178499151HCID 178499151, Verbindung

Produkt 1

HCID 178499150HCID 178499150, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
44 °C

Versuchsvorschrift

To a solution of Intermediate 1D (0.94 g, 3.24 mmol) in DCM (30 mL) was added thionyl chloride (0.95 mL, 12.96 mmol). The resulting mixture was stirred at 44° C. overnight and allowed to cool to ambient temperature. The mixture was concentrated under reduced pressure, azeotroped with acetonitrile and dried under vacuum overnight to give Intermediate 1E in quantitative yield as a white solid which was used in the next step without further purification.

Aufarbeitung

  1. temperatureto cool to ambient temperature
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customazeotroped with acetonitrile
  4. customdried under vacuum overnight

Quellen und Nachweise

ORD-Eintrag
ord-a4a7fa5c47c54e858cca29ded96a9d57
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08431565B2

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