反応 #6915

ord-5899155eb2234a2e8997519924de4408

反応条件

温度
20°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled in an ice bath
  2. 2
    その他partitioned between ethyl acetate and sodium thiosulphate
  3. 3
    その他The organic phase was dried
  4. 4
    濃縮concentrated in vacuo

実験手順

7-Amino-quinazolin-4-one (R. Dempsy and E. Skito, Biochemistry, 30, 1991, 8480) (1.61 g) was suspended in 6N HCl (20 ml) and cooled in an ice bath. A solution of sodium nitrite (0.75 g) in water (10 ml) was added dropwise over 15 minutes. After a further 10 minutes, a solution of potassium iodide (1.66 g) in water (5 ml) was added dropwise. The mixture was warmed to 20° C. and after 3 hours partitioned between ethyl acetate and sodium thiosulphate. The organic phase was dried and concentrated in vacuo to give the title compound (0.485 g); m/z (M+1+) 271.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07084147B2uspto-grants-2006_08