Aluminum(III) Chloride → HCID 68676527, Verbindung

HRID 2233018Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2233018
C([N:5]1[C:18](=[O:19])[N:8]2[CH:9]=[C:10]([C:14]([CH3:17])([CH3:16])[CH3:15])[N:11]=[C:12]([Cl:13])[C:7]2=[N:6]1)(C)(C)C.[Cl-].[Cl-].[Cl-].[Al+3]>ClCCCl>[C:14]([C:10]1[N:11]=[C:12]([Cl:13])[C:7]2[N:8]([C:18](=[O:19])[NH:5][N:6]=2)[CH:9]=1)([CH3:17])([CH3:15])[CH3:16]

Komponenten

4

Edukt 2

HCID 6451240Aluminum(III) ChlorideHCID 68678410HCID 68678410, Verbindung

Produkt 1

HCID 68676527HCID 68676527, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A solution of 4.10 g of the product of Step E in 1,2-dichloroethane (142 mL) was treated with 5.60 g of aluminum trichloride and the suspension was heated to 80° C. After two h, the reaction mixture was cooled to ambient temperature and poured into ice water (500 g). After the ice had dissolved, the mixture was extracted with EtOAc and the organic layer was washed with sat. sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography to afford 6-tert-butyl-8-chloro-2H-[1,2,4]triazolo[4,3-a]pyrazin-3-one as a yellow solid. MS (M+H+)=227.3.

Aufarbeitung

  1. temperatureAfter two h, the reaction mixture was cooled to ambient temperature
  2. extractionthe mixture was extracted with EtOAc
  3. washthe organic layer was washed with sat. sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-aca4f55900ba465889a136bd4e5c9cf8
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07709473B2

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