Phosphorus oxychloride → 4-Tert-butyl-6-chloropyrimidin-2-amine

HRID 617782ノート

反応式

HRID 617782 の反応式
[NH2:1][C:2]1[N:7]=[C:6](O)[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[NH2:1][C:2]1[N:7]=[C:6]([Cl:15])[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[N:3]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178441204HCID 178441204、化合物

生成物 1

HCID 218463784-Tert-butyl-6-chloropyrimidin-2-amine

実験手順

2-Amino-4-hydroxy-6-tert-butylpyrimidine (8.35 g) was dissolved in 50 mL of phosphorus oxychloride and the solution refluxed for 2 hours. Excess phosphorus oxychloride was removed under vacuum and the residue dissolved in 100 mL of ethanol. The solution was adjusted to pH 8 with ice-cold concentrated ammonium hydroxide, and solvent removed under reduced pressure. The residue was filtered to give a white solid, which was recrystallized from ethanol-water to give 2-amino-4-chloro-6-tert-butylpyrimidine (3.66 g), m.p. 87.7-88.90° C.

後処理

  1. temperaturethe solution refluxed for 2 hours
  2. customExcess phosphorus oxychloride was removed under vacuum
  3. dissolutionthe residue dissolved in 100 mL of ethanol
  4. customremoved under reduced pressure
  5. filtrationThe residue was filtered
  6. customto give a white solid, which
  7. customwas recrystallized from ethanol-water

出典と根拠

ORDレコード
ord-99e6e0411197410d89d6f00a4595dbde
出典データセット
uspto-grants-1999_09
特許番号
US05952331

反応ノート

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