反応 #4007

反応方程式

2-amino-4-chloromethyl-6-methoxypyrimidine

caesium fluoride

→

2-amino-4-fluoromethyl-6-methoxypyrimidine

溶媒

dimethylformamide

反応条件

後処理

1. 1
   温度under reflux for 2 hours
2. 2
   温度The mixture was cooled
3. 3
   その他evaporated in vacuo
4. 4
   洗浄the solution was washed four times with water
5. 5
   乾燥The organic phase was dried with anhydrous magnesium sulphate
6. 6
   workup.STIRRINGstirred with decolourising charcoal
7. 7
   ろ過filtered
8. 8
   その他evaporated
9. 9
   その他The crude product was purified by chromatography on silica
10. 10
    洗浄eluted with ethyl acetate

実験手順

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.

出典