反应 #1435736

ord-b8fc64842d254a7a9cabb6ac7f48d28c

反应方程式

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
收率 47.7%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooling
  2. 2
    洗涤The separated organic layer was washed with water
  3. 3
    干燥dried over sodium sulfate
  4. 4
    浓缩concentrated

实验过程

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.

来源

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