2-Amino-4-chloropyrimidine → 4-Methoxy-2-pyrimidinamine

HRID 872296

反応式

HRID 872296 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[N:3]=1.[CH3:9][O-:10].[Na+]>CO>[CH3:9][O:10][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[N:3]=1

参加物

4

実験手順

A solution of 4-chloro-pyrimidin-2-ylamine (10 g, 77 mmol) in methanol (400 mL) under argon, was treated with a solution of sodium methoxide in methanol (25.7%, 51.59 mL, 0.232 mol) whereupon a cream yellow solution was obtained. The reaction was heated at reflux for 3 hours to give a clear yellow green solution. On cooling the volatiles were removed in vacuo and the residue taken up in 100 mL EtOAc and washed with 100 mL water. The organic phase was dried, filtered and concentrated in vacuo to give the title compound as a white solid (9.12 g).

後処理

  1. customwas obtained
  2. temperatureThe reaction was heated
  3. temperatureat reflux for 3 hours
  4. customto give a clear yellow green solution
  5. temperatureOn cooling the volatiles
  6. customwere removed in vacuo
  7. washwashed with 100 mL water
  8. customThe organic phase was dried
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c192c0921800477bb0d096d57c361c97
出典データセット
uspto-grants-2015_03
特許番号
US08975265B2

関連ノート

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