反应详情

Pyridine was added to a suspension of C-[2-Amino-6-(2,4-dimethylphenyl)-5-formyl-pyrimidin-4-ylsulphanyl]-N-cyclopropyl-methane sulphonamide in dichloromethane and the mixture cooled, ice/water. Trifluoroacetic anhydride was added and the mixture stirred for ˜2 hrs and heated under reflux for ˜24 hrs. The resulting dark red solution was allowed to cool and aqueous ammonia (0.880) added and the mixture stirred for ˜30 mins. Dichloromethane was added and the mixture washed with dilute hydrochloric acid, water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a red/orange solid. The crude solid was purified by preparative HPLC.

1. temperaturethe mixture cooled
2. temperatureheated
3. temperatureunder reflux for ˜24 hrs
4. temperatureto cool
5. stirringthe mixture stirred for ˜30 mins
6. washthe mixture washed with dilute hydrochloric acid, water and saturated aqueous sodium chloride solution
7. dry with materialThe solution was dried over anhydrous sodium sulphate
8. concentrationconcentrated to a red/orange solid
9. customThe crude solid was purified by preparative HPLC