反应详情

6.59 g (19 mM) of xanthine and 5.07 g (22.8 mM) of phosphorus pentasulfide were heated under reflux in 102 ml of pyridine for 3 days. At 0° C., 25.1 ml of 2N NaOH were added. The solid was filtered off and washed with pyridine. The solvents were evaporated in vacuo, the residue suspended in water, collected, redissolved in 100 ml of 1N NaOH and 50 ml of isopropanol, treated twice with 0.3 g of charcoal, filtered and neutralized with 5N HCl to pH 7. The isopropanol was removed in vacuo and the solid collected, washed and dried to give 6.80 g (98.7%) of 6-thioxanthine, mp 188-9° C.

1. filtrationThe solid was filtered off
2. washwashed with pyridine
3. customThe solvents were evaporated in vacuo
4. customcollected
5. dissolutionredissolved in 100 ml of 1N NaOH
6. addition50 ml of isopropanol, treated twice with 0.3 g of charcoal
7. filtrationfiltered
8. customThe isopropanol was removed in vacuo
9. customthe solid collected
10. washwashed
11. customdried