Cesium fluoride → 2-Amino-4-fluoromethyl-6-methoxypyrimidine
반응식
[NH2:1][C:2]1[N:7]=[C:6]([CH2:8]Cl)[CH:5]=[C:4]([O:10][CH3:11])[N:3]=1.[F-:12].[Cs+]>CN(C)C=O>[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][F:12])[CH:5]=[C:4]([O:10][CH3:11])[N:3]=1참가 물질
4
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.
후처리
- temperatureunder reflux for 2 hours
- temperatureThe mixture was cooled
- customevaporated in vacuo
- washthe solution was washed four times with water
- dry with materialThe organic phase was dried with anhydrous magnesium sulphate
- stirringstirred with decolourising charcoal
- filtrationfiltered
- customevaporated
- customThe crude product was purified by chromatography on silica
- washeluted with ethyl acetate
출처 및 근거
- ORD 기록
- ord-57c87955e9ed4a11aa4e6f98c7716c2b
- 출처 데이터셋
- uspto-grants-1988_02
- 특허 번호
- US04723006
반응 노트
불러오는 중…