반응 #73849

반응 방정식

2-Bromopyridine

ethyl bromodifluoroacetate

isopropyl acetate

→

Ethyl difluoro(pyridin-2-yl)acetate

용매

DMF

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to RT
2. 2
   기타The reaction mixture was quenched with the aqueous potassium dihydrogen phosphate at 0-10° C.
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   여과The reaction mixture was filtered off
5. 5
   기타the residue obtained
6. 6
   세척was washed with ethyl acetate
7. 7
   기타The organic layer was collected
8. 8
   세척washed with brine solution
9. 9
   건조dried over sodium sulphate
10. 10
    workup.DISTILLATIONthen distilled under vacuum

실험 절차

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).

출처