Reaktion #1955
ord-1ecb12c0a720485081b2a903dedaad68
Reaktionsgleichung
water
4-chloro-5-fluoro-2-picoline
product
4-Chloro-5-fluoro-2-picoline
t-butylhypochlorite
→
title compound
3,4-Dichloro-5-fluoro-2-picoline
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Extraktionthe resultant aqueous mixture is extracted with methylene chloride
- 2TrocknenThe organic solution is dried over anhydrous magnesium sulfate
- 3Filtrationfiltered
- 4Einengenconcentrated under reduced pressure
- 5workup.DISTILLATIONdistilled
Vorschrift
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.