반응 #1435736

ord-b8fc64842d254a7a9cabb6ac7f48d28c

반응 방정식

O=C(O)CC(O)(CC(=O)O)C(=O)O
citric acid
Fc1cc(F)c(-c2c(Cl)nc3nccn3c2Cl)c(F)c1
5,7-dichloro-6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidine
Cc1cc(C)[nH]n1
3,5-dimethylpyrazole
[H-].[Na+]
sodium hydride
Cc1cc(C)n(-c2c(-c3c(F)cc(F)cc3F)c(Cl)nc3nccn23)n1
5-(3,5-dimethylpyrazol-1-yl)-6-(2,4,6-trifluorophenyl)-7-chloroimidazo[1,2-a]pyrimidine
수율 47.7%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    세척The separated organic layer was washed with water
  3. 3
    건조dried over sodium sulfate
  4. 4
    농축concentrated

실험 절차

Into a mixture of 0.040 g of sodium hydride (60% in oil) and 2 ml of tetrahydrofuran, a solution of 0.096 g of 3,5-dimethylpyrazole in 3 ml of tetrahydrofuran was added dropwise. The mixture was added to a solution of 0.32 g of 5,7-dichloro-6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidine in 5 ml of tetrahydrofuran under ice-cooling. To the reaction mixture, chloroform and aqueous citric acid solution were added. The separated organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was subjected to silica gel column chromatography to give 0.18 g of 5-(3,5-dimethylpyrazol-1-yl)-6-(2,4,6-trifluorophenyl)-7-chloroimidazo[1,2-a]pyrimidine.

출처

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