反応 #69007

ord-65f397ec3e8d46fcb30e760fe36cae26

反応条件

温度
75°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled
  2. 2
    その他The layers were separated
  3. 3
    抽出the aqueous layer was extracted with EtOAc (4×)
  4. 4
    乾燥The combined organics were dried (MgSO4)
  5. 5
    濃縮concentrated
  6. 6
    その他to give a near colorless solid which
  7. 7
    その他was used without further purification

実験手順

To a solution 2-chloro-4-methoxypyrimidine (2 g, 13.8 mmol) in ethoxyethanol (50 mL) was added 4-(3-methyl-1H-1,2,4-triazol-1-yl)aniline (1.7 g, 10.6 mmol). The reaction was warmed to 75° C. for 16 h, cooled, and diluted with water and EtOAc. The layers were separated, and the aqueous layer was extracted with EtOAc (4×). The combined organics were dried (MgSO4), and concentrated to give a near colorless solid which was homogeneous by analytical HPLC analysis and was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530480B2uspto-grants-2013_09