preparation | the preparation of p-pyridyl thiourea is as follows: 1, 1-thiocarbonyldiimidazole (29.4g,0.16mol) was added to a solution of 4-aminopyridine (14.1g,0.15mol) in dry tetrahydrofuran (ML) and the resulting mixture was stirred for 17 hours. The solvent was removed under reduced pressure and the resulting solid was suspended in a mixture of dichloromethane and water. The undissolved solid was filtered and then washed with acetone to give the solid product (8.98g). Gaseous ammonia was bubbled through a solution of the resulting solid product (8.50g,0.06mol) in anhydrous tetrahydrofuran (ml) for 20 min. The ammonia flow was stopped and the mixture was stirred for 17 hours during which time a precipitate formed in the reaction. Filtration followed by drying of the solid under vacuum gave the desired thiourea product P-pyridylthiourea (5.1g). |