Reacción #73849

Ecuación de reacción

2-Bromopyridine

ethyl bromodifluoroacetate

isopropyl acetate

→

Ethyl difluoro(pyridin-2-yl)acetate

Disolventes

DMF

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe reaction mixture was cooled to RT
2. 2
   OtroThe reaction mixture was quenched with the aqueous potassium dihydrogen phosphate at 0-10° C.
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   FiltraciónThe reaction mixture was filtered off
5. 5
   Otrothe residue obtained
6. 6
   Lavadowas washed with ethyl acetate
7. 7
   OtroThe organic layer was collected
8. 8
   Lavadowashed with brine solution
9. 9
   Secadodried over sodium sulphate
10. 10
    workup.DISTILLATIONthen distilled under vacuum

Procedimiento

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).

Fuente