Reaktion #73849

Reaktionsgleichung

2-Bromopyridine

ethyl bromodifluoroacetate

isopropyl acetate

→

Ethyl difluoro(pyridin-2-yl)acetate

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was cooled to RT
2. 2
   SonstigeThe reaction mixture was quenched with the aqueous potassium dihydrogen phosphate at 0-10° C.
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   FiltrationThe reaction mixture was filtered off
5. 5
   Sonstigethe residue obtained
6. 6
   Waschenwas washed with ethyl acetate
7. 7
   SonstigeThe organic layer was collected
8. 8
   Waschenwashed with brine solution
9. 9
   Trocknendried over sodium sulphate
10. 10
    workup.DISTILLATIONthen distilled under vacuum

Vorschrift

2-Bromopyridine (20 g), ethyl bromodifluoroacetate (27.2 g) and DMF (120 mL) were added and stirred for 10 minutes under nitrogen. Copper powder was added to the reaction mixture and heated to 70-80° C. for 45 minutes. The reaction mixture was cooled to RT and 400 mL of isopropyl acetate (IPAc) was added. The reaction mixture was quenched with the aqueous potassium dihydrogen phosphate at 0-10° C. and stirred for 30 minutes. The reaction mixture was filtered off and the residue obtained was washed with ethyl acetate. The organic layer was collected and washed with brine solution and dried over sodium sulphate then distilled under vacuum. (Crude weight=20 g).

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