Phosphorus oxychloride → 7-Chloro-1-ethyl-1H-pyrazolo[4,3-d]pyrimidine

HRID 573345ノート

反応式

HRID 573345 の反応式
[CH2:1]([N:3]1[C:11]2[C:10](O)=[N:9][CH:8]=[N:7][C:6]=2[CH:5]=[N:4]1)[CH3:2].O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:10]1[C:11]2[N:3]([CH2:1][CH3:2])[N:4]=[CH:5][C:6]=2[N:7]=[CH:8][N:9]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178463033HCID 178463033、化合物

生成物 1

HCID 714458087-Chloro-1-ethyl-1H-pyrazolo[4,3-d]pyrimidine

反応条件

温度
100 °C

実験手順

A mixture of 1-ethyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol (2.91 g) and POCl3 (30 mL) was stirred at 100° C. overnight. The mixture was concentrated under reduced pressure. The residue was neutralized with saturated NaHCO3 aqueous solution and extracted with AcOEt. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (2.14 g).

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. extractionextracted with AcOEt
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (AcOEt/hexane)

出典と根拠

ORDレコード
ord-dfa8156422914e4a99cd25b0ab75f904
出典データセット
uspto-grants-2015_05
特許番号
US09029536B2

反応ノート

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