Phosphorus oxychloride → 5,7-Dichloro-[1,2,4]triazolo[1,5-c]pyrimidine

HRID 2389766ノート

反応式

HRID 2389766 の反応式
[Cl:1][C:2]1[N:7]=[C:6](O)[N:5]2[N:9]=[CH:10][N:11]=[C:4]2[CH:3]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[N:5]2[N:9]=[CH:10][N:11]=[C:4]2[CH:3]=[C:2]([Cl:1])[N:7]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178517804HCID 178517804、化合物

生成物 1

HCID 552791785,7-Dichloro-[1,2,4]triazolo[1,5-c]pyrimidine

反応条件

温度
120 °C

実験手順

927 mg (4.19 mmol) of 7-chloro[1,2,4]triazolo[1,5-c]pyrimidin-5-ol (Example 52A) are suspended in 16.9 g (110.13 mmol) of phosphoryl chloride under argon and heated at 120° C. for 4 h. After this time, the excess phosphoryl chloride is removed in vacuo, and the residue is distilled together with toluene. The residue is suspended in water, the pH is brought to 7 with saturated aqueous sodium bicarbonate solution, and the precipitated solid is filtered off with suction. The latter is washed with water and dried over phosphorus pentoxide for 18 h. 389 mg (49% of theory) of the product are obtained.

後処理

  1. customAfter this time, the excess phosphoryl chloride is removed in vacuo
  2. distillationthe residue is distilled together with toluene
  3. filtrationthe precipitated solid is filtered off with suction
  4. washThe latter is washed with water
  5. dry with materialdried over phosphorus pentoxide for 18 h
  6. custom389 mg (49% of theory) of the product are obtained

出典と根拠

ORDレコード
ord-a4b39178bc684441afe6712af9b378e3
出典データセット
uspto-grants-2012_09
特許番号
US08273752B2

反応ノート

読み込み中…