反応 #1435725

ord-3548f248f23c401e85b4ee7b9c5386b4

反応方程式

CCOC(=O)C(C(=O)OCC)c1c(F)cc(F)cc1F
diethyl (2,4,6-trifluorophenyl)malonate
Cl.Nc1ncc[nH]1
2-aminoimidazole hydrochloride
C1CCC2=NCCCN2CC1
DBU
CN(C)C=O
N,N-dimethylformamide
Oc1nc2nccn2c(O)c1-c1c(F)cc(F)cc1F
5,7-dihydroxy-6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidine
収率 78.3%

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    濃縮The separated water layer was concentrated
  3. 3
    workup.ADDITIONthe residue was diluted with water and conc. hydrochloric acid
  4. 4
    workup.ADDITIONwas added
  5. 5
    温度under ice-cooling
  6. 6
    その他The precipitation
  7. 7
    ろ過was filtered
  8. 8
    その他dried

実験手順

A mixture of 2.90 g of diethyl (2,4,6-trifluorophenyl)malonate, 2.39 g of 2-aminoimidazole hydrochloride, 4.57 g of DBU and 10 ml of N,N-dimethylformamide was heated at 100° C. for 6 hours. After allowing the reaction mixture to cool to room temperature, chloroform and water were added thereto. The separated water layer was concentrated, the residue was diluted with water and conc. hydrochloric acid was added thereto under ice-cooling. The precipitation was filtered and dried to give 2.2 g of 5,7-dihydroxy-6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidine.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07211545B2uspto-grants-2007_05