Reaktion #1435736

ord-b8fc64842d254a7a9cabb6ac7f48d28c

Reaktionsgleichung

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
Ausbeute 47.7%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    WaschenThe separated organic layer was washed with water
  3. 3
    Trocknendried over sodium sulfate
  4. 4
    Einengenconcentrated

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07211545B2uspto-grants-2007_05