1. ) 2 (64.1 mg, 0.12 mmol) and (Ph 2 PO) 2 NH (100.00 mg, 0.24 mmol) were stirred together in 15 ml of dry THF and refluxed for 18 hours. The reaction mixture was filtered and evaporated to dryness. The crude compound was recrystallised from toluene yielding colourless blocks of 4.C 7 H 8;Yield = 135.8 mg (81 %), FT-IR (ATR/cm -1 ) 3052(w), 3011(w), 1438 (s), 1211 (vs,PNP), 1180 (s,PNP), 1124 (vs, PO), 1086 (vs, PO), 1064 (s)
2. mg, 0.24 mmol) were stirred together in 15 ml of dry THF and refluxed for 18 hours. The reaction mixture was filtered and evaporated to dryness. Colourless blocks of 5. were grown from a solution in acetonitrile. Yield = 142.3 mg (85 %), 31 P{ 1 H} NMR (162 MHz,CDCl 3 ) ? 24;FT-IR (ATR/cm -1 ) 3052(w), 2924(w), 1437(s), 1208 (s, PNP), 1175 (s, PNP), 1122 (s, PO), 1083 (s, PO), 1062 (s), 1025 (s), 998 (s), 852(s), 811(s), 752 (s)
3. mg, 0.24 mmol) in 15 ml of dry THF were refluxed for 18 hours with constant stirring. The reaction mixture was filtered and evaporated to dryness. The reaction mixture was filtered and evaporated to dryness giving a pale pink colored solid;The solid was recrystallized from acetonitrile Yield = 139 mg (83 %), 31 P{ 1 H} NMR (162 MHz, CDCl 3 ) ? 18.4, FT-IR (ATR/cm -1 ) 3054(w), 3012(w), 2925(w), 2854(w), 1437(s), 1217(s, PNP), 1195(PNP), 1174 (PNP), 1122 (s, PO)