Water → 3,4-Dichloro-5-fluoro-2-picoline

HRID 1450065

Reaktionsgleichung

Reaktionsgleichung von HRID 1450065
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]([CH3:9])[CH:3]=1.C(O[Cl:15])(C)(C)C.O>C(Cl)(Cl)Cl>[Cl:15][C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[C:7]([F:8])[C:2]=1[Cl:1]

Komponenten

5

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To 0.87 g (6 mmol) of 4-chloro-5-fluoro-2-picoline, the product of Example 66, in 20 mL of chloroform cooled to -45° C., is added 0.75 mL of t-butylhypochlorite. The reaction mixture is stirred at -45° C. for 2 hours and at 0° C. for 2 hours. The reaction mixture is then poured into water and the resultant aqueous mixture is extracted with methylene chloride. The organic solution is dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure and distilled to afford the title compound.

Aufarbeitung

  1. extractionthe resultant aqueous mixture is extracted with methylene chloride
  2. dry with materialThe organic solution is dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-014f44cb018147659fc5b134765083b2
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05599816

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