反应详情

A mixture of the above 5-cycloheptyl-6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidin-7-ol (294 mg) in 2 mL of phosphorous oxychloride is heated at reflux for 6 h. The excess phosphorous oxychloride is removed in vaccuo, and the resulting residue is dissolved in methylene chloride. The organic layer is washed with water, dried over magnesium sulfate, and concentrated. The residue is chromatographed over silica gel, eluting with a gradient of 10% ethyl acetate in hexanes to 33% ethyl acetate in hexanes. Concentration provides 7-chloro-5-cycloheptyl-6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidine as a white solid (24 mg). MS: m/z 380.2 (M+H).

1. temperatureis heated
2. temperatureat reflux for 6 h
3. customThe excess phosphorous oxychloride is removed in vaccuo
4. dissolutionthe resulting residue is dissolved in methylene chloride
5. washThe organic layer is washed with water
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated
8. customThe residue is chromatographed over silica gel
9. washeluting with a gradient of 10% ethyl acetate in hexanes to 33% ethyl acetate in hexanes
10. concentrationConcentration