Phosphorus oxychloride → 4-Chloropyrido[2,3-d]pyrimidine

HRID 1086999

反応式

HRID 1086999 の反応式
[N:1]1[C:6]2[N:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4](=O)[NH:3][CH:2]=1.O=P(Cl)(Cl)[Cl:14]>>[Cl:14][C:4]1[C:5]2[CH:10]=[CH:9][CH:8]=[N:7][C:6]=2[N:1]=[CH:2][N:3]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 1354402774-Hydroxypyrido (2,3-d)pyrimidine

生成物 1

HCID 5690394-Chloropyrido[2,3-d]pyrimidine

実験手順

A mixture of 17.8 g of Pyrido[2,3-d]pyrimidin4(3H)one and 200 mL of POCl3 was stirred under reflux for one hour. Excess POCl3 was removed under vacuum, and then CH2Cl2, ice, and water were added. A black solid dissolved slowly. The organic layer was then separated, washed with aqueous NaHCO3, and dried over Na2SO4. Solvent was then removed under vacuum to leave a yellow solid, which was recrystallized from toluene/hexane. M.P. 137° dec.

後処理

  1. temperatureunder reflux for one hour
  2. customExcess POCl3 was removed under vacuum
  3. additionCH2Cl2, ice, and water were added
  4. dissolutionA black solid dissolved slowly
  5. customThe organic layer was then separated
  6. washwashed with aqueous NaHCO3
  7. dry with materialdried over Na2SO4
  8. customSolvent was then removed under vacuum
  9. customto leave a yellow solid, which
  10. customwas recrystallized from toluene/hexane

出典と根拠

ORDレコード
ord-92255a965cad4addb14d89dee2ad5945
出典データセット
uspto-grants-1991_07
特許番号
US05034393

関連ノート

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