반응 #1435725

ord-3548f248f23c401e85b4ee7b9c5386b4

반응 방정식

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
수율 78.3%

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool to room temperature
  2. 2
    농축The 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
    온도under ice-cooling
  6. 6
    기타The precipitation
  7. 7
    여과was filtered
  8. 8
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07211545B2uspto-grants-2007_05