P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].C(=O)(O)[O-].[Na+].COCCOCCOC.[C:29]1([C:35]2[NH:44][C:38]3[N:39]=[CH:40][N:41]=[C:42](O)[C:37]=3[CH:36]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>O>[C:29]1([C:35]2[NH:44][C:38]3[N:39]=[CH:40][N:41]=[C:42]([SH:2])[C:37]=3[CH:36]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
After adding 6.19 g of phosphorus pentasulfide, 6.24 g of sodium bicarbonate and 25 ml of diglyme to 2.45 g of the 6-phenyl-7H-pyrrolo[2,3-d]pyrimidin-4-ol described in WO97/02266 and PCT/EP96/02728, and stirring the mixture for 1 hour, an additional 3 g of phosphorus pentasulfide and 3 g of sodium bicarbonate were added and the mixture was stirred for 1 hour. There were further added another 3 g of phosphorus pentasulfide and 3 g of sodium bicarbonate, and the mixture was stirred for 1 hour. It was then returned to room temperature, water was added, the mixture was stirred for 10 minutes, and the precipitated crystals were filtered out, washed with water and dried to obtain 2.5 g of the title compound.
Loading…
