抄録
A comparative study was carried out on the reaction products of phosphoryl chloride and ammonia (phosphoryl amides) in a conventional solvent, ethyl ether, and in methanol saturated with ammonia. In ethyl ether, amide-substituted products were practically insoluble in the solvent, thus the reaction mixture became slurry in the course of the reaction and the complete substitution of amide for chlorine was difficult, while in the ammonia-saturated solution, the reaction products were almost soluble in the solvent and more than 90% of reaction products was phosphoryl triamide. While phosphoryl triamide and ammonium chloride (a by-product of the reaction) have low solubility in both solvents, methanol and liquid ammonia, the ammonia-saturated methanol was a good solvent for both phosphoryl triamide and ammonium chloride. Although the reaction of methanol with phosphoryl chloride proceeded vigorously even at lower temperatures, only a very small amount of methoxy-substituted products were detected in the reaction mixture by use of the ammonia-saturated solution. Therefore, the ammonia-satu-rated methanol was very suitable for the preparation of phosphoryl triamide for shrink-proof finish of rayon and silk.
