Acetonitrile → HCID 86703140, Verbindung

HRID 2410123Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2410123
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]=[C:4](Cl)[CH:3]=1.S([O:16][CH3:17])(OC)(=O)=O.C(#N)C.C([O-])(O)=O.[Na+]>C(Cl)Cl>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]([CH3:4])[C:17](=[O:16])[CH:3]=1

Komponenten

6

Edukt 4

HCID 6342AcetonitrileHCID 6497Dimethyl SulfateHCID 516892Sodium BicarbonateHCID 467387064-Bromo-2-chloro-5-methoxypyridine

Produkt 1

HCID 86703140HCID 86703140, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 4-bromo-2-chloro-5-methoxypyridine (1 g, 4.5 mmol) in dimethyl sulfate (1.9 mL, 19.5 mmol) was stirred at 120° C. for 16 h in a sealed tube. After cooling, acetonitrile and a saturated aqueous NaHCO3 solution were added and the mixture was stirred at rt over week-end. DCM was added and extracted. The organic layer was dried (Na2SO4), filtered and concentrated to give the title compound. tR: 0.57 min (LC-MS 2); ESI-MS: 218.0/220.0 [M+H]+ (LC-MS 2).

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-485e28b23245410b82806ecaab39fd7e
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08815926B2

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