Phosphorus sulfide (P2S5) → HCID 178504191, compound

Participants

Reaction Steps

In a flask were placed 2.90 g (0.0105 mole) of 3-amino-5-hydroxy-6-(4-methyl-4-phenyl-4-silapentyl)-1,2,4-triazine, 8.94 g (0.0201 mole) of phosphorus pentasulfide, and 40 mL of pyridine. This mixture was heated at reflux under a nitrogen atmosphere for one hour. The reaction mixture was concentrated under reduced pressure to a volume of approximately 25 mL and then mixed with 150 mL of ice water. The resulting mixture was warmed on a steam bath for 4 hours after which it was cooled to ambient temperature. An orange solid was collected from this mixture by filtration and was stirred with 60 mL of methanol. Filtration of this mixture yielded 2.70 g of 3-amino-5-mercapto-6-(4-methyl-4-phenyl-4-silapentyl)-1,2,4-triazine, m.p. 255°-257° C. (decomposition). The NMR and IR spectra were consistent with the proposed structure.

Provenance & Evidence