反応 #1435736

ord-b8fc64842d254a7a9cabb6ac7f48d28c

反応方程式

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
収率 47.7%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooling
  2. 2
    洗浄The separated organic layer was washed with water
  3. 3
    乾燥dried over sodium sulfate
  4. 4
    濃縮concentrated

実験手順

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.

出典

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