CYCLOTRIPHOSPHAZENE-PMMH-6 DENDRIMER GENERATION 0.5 synthesis
- Product Name:CYCLOTRIPHOSPHAZENE-PMMH-6 DENDRIMER GENERATION 0.5
- CAS Number:77958-57-7
- Molecular formula:C42H30N3O12P3
- Molecular Weight:861.6218
123-08-0
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Yield:77958-57-7 96.9%
Reaction Conditions:
with 2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine;potassium carbonate in tetrahydrofuran at 20; for 24 h;Inert atmosphere;
Steps:
Synthesis of [N3P3(O12C42H30)] (compound 6)
A mixture of N3P3Cl6 (1.00 g, 2.88 mmol), K2CO3 (3.94 g,28.48 mmol) and 4-oxybenzaldehyde (2.32 g, 18.99 mmol)was stirred in anhydrous THF (100 mL) under nitrogenatmosphere at room temperature for 24 h. The reaction wasmonitored by 31P NMR until a new single appeared. Thereaction mixture was centrifuged and the solvent wasremoved under reduced pressure, the crude product waspurified by recrystallized with petroleum ether and dichloromethane.The spectra is consistent with that in the literature.[33] White solid (1.63 g, 96.9%). 1H NMR (400 MHz,CDCl3) d/ppm 9.96 (s, 6H), 7.76 (d, 12H, J8.4 Hz), 7.17(d, 12H, J8.4 Hz). 31P NMR (162 MHz, CDCl3): d 7.08.13C NMR (100 MHz, CDCl3) d 190.29, 154.51, 133.82,131.95, 131.35, 121.22.
References:
Chen, Jipeng;Wang, Le;Yang, Yunxia;Xu, Mengsheng;Xie, Jinhua;Liu, Pan [Phosphorus, Sulfur and Silicon and the Related Elements,2020,vol. 196,# 1,p. 79 - 85]
22666-84-8
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