Cesium fluoride → 2-Amino-4-fluoromethyl-6-methoxypyrimidine

HRID 3911

反応式

HRID 3911 の反応式
[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]=1

参加物

4

反応物 2

HCID 25953Cesium fluorideHCID 138848154-(Chloromethyl)-6-methoxypyrimidin-2-amine

生成物 1

HCID 201534972-Amino-4-fluoromethyl-6-methoxypyrimidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

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.

後処理

  1. temperatureunder reflux for 2 hours
  2. temperatureThe mixture was cooled
  3. customevaporated in vacuo
  4. washthe solution was washed four times with water
  5. dry with materialThe organic phase was dried with anhydrous magnesium sulphate
  6. stirringstirred with decolourising charcoal
  7. filtrationfiltered
  8. customevaporated
  9. customThe crude product was purified by chromatography on silica
  10. washeluted with ethyl acetate

出典と根拠

ORDレコード
ord-57c87955e9ed4a11aa4e6f98c7716c2b
出典データセット
uspto-grants-1988_02
特許番号
US04723006

関連ノート

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