反应详情

A 1000-mL stirrer-equipped autoclave was charged with 40.0 g (0.041 mol) of hexakis(4-nitrophenoxy)cyclotriphosphazene (2), aniline (75 mL), and 0.1 g of PtO2 catalyst. The mixture was agitated vigorously under 50 psi of hydrogen pressure at 50° C. until no further pressure drop was recorded (~30 h). The reaction mixture was filtered and the filtrate was poured slowly into toluene (1000 mL). Impure 3 precipitated from solution. After filtration, the crude 3 was recrystallized from o-dichlorobenzene and from THF to yield 30 g (92%) of pure 3, mp 189°-190° C. A 31P NMR spectrum in THF showed a singlet at 11.2 ppm, which indicated complete conversion of NO2 to NH2 groups.

1. customA 1000-mL stirrer-equipped autoclave
2. custom(~30 h)
3. filtrationThe reaction mixture was filtered
4. additionthe filtrate was poured slowly into toluene (1000 mL)
5. customImpure 3 precipitated from solution
6. filtrationAfter filtration
7. customthe crude 3 was recrystallized from o-dichlorobenzene and from THF
8. customto yield 30 g (92%) of pure 3, mp 189°-190° C