반응 #4007

반응 방정식

2-amino-4-chloromethyl-6-methoxypyrimidine

caesium fluoride

→

2-amino-4-fluoromethyl-6-methoxypyrimidine

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도under reflux for 2 hours
2. 2
   온도The mixture was cooled
3. 3
   기타evaporated in vacuo
4. 4
   세척the solution was washed four times with water
5. 5
   건조The organic phase was dried with anhydrous magnesium sulphate
6. 6
   workup.STIRRINGstirred with decolourising charcoal
7. 7
   여과filtered
8. 8
   기타evaporated
9. 9
   기타The crude product was purified by chromatography on silica
10. 10
    세척eluted with ethyl acetate

실험 절차

A mixture of 17.0 parts of 2-amino-4-chloromethyl-6-methoxypyrimidine, 59.5 parts of caesium fluoride and 130 parts of dry dimethylformamide was stirred under reflux for 2 hours. The mixture was cooled and evaporated in vacuo. The residue was taken up in ethyl acetate and the solution was washed four times with water. The organic phase was dried with anhydrous magnesium sulphate, stirred with decolourising charcoal, filtered and evaporated. The crude product was purified by chromatography on silica, eluted with ethyl acetate to give 2-amino-4-fluoromethyl-6-methoxypyrimidine m.p. 119°-121° C.

출처