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

HRID 2234833ノート

反応式

HRID 2234833 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.O=P(Cl)(Cl)[Cl:14]>>[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

実験手順

The mixture of 7-Chloro-[1,2,4]triazolo[1,5-c]pyrimidin-5-ol (35 mg) in POCl3 was heated at reflux for 3 hours. After removal of the volatiles, the residue was purified by a short plug column eluting with 1:1 EtOAc/hexane to give 5,7-Dichloro-[1,2,4]triazolo[1,5-c]pyrimidine as an off-white solid (11 mg). 1H NMR (400 MHz, CDCl3) δ 8.49 (s, 1H) 7.72 (s, 1H). [M+H] calc'd for C5H2Cl2N4, 189; found, 189.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customAfter removal of the volatiles
  4. customthe residue was purified by a short plug column
  5. washeluting with 1:1 EtOAc/hexane

出典と根拠

ORDレコード
ord-be29e2cf6318409b916d88cf8035f974
出典データセット
uspto-grants-2010_05
特許番号
US07713973B2

反応ノート

読み込み中…