Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Monobenzone | HCID 7638 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Hexachlorocyclotriphosphazene | HCID 220225 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 101742540 | HCID 101742540 | — |
Reaction Steps
A suspension of 20.00 g (5.74×10-2 mol) of hexachlorocyclotriphosphazene, 22.99 g (0.57 mol) of NaH 60% oil dispersion, and 1.5 g of tetrabutylammonium bromide in 200 mL of THF is treated with 115.1 g (0.57 mol) of 4-(benzyloxy)phenol in 250 mL of THF. This treatment is performed dropwise, waiting each time for hydrogen evolution. The reaction mixture is successively refluxed for 48 hrs, cooled to room temperature, and ultracentrifuged at 8000 rpm to separate the liquid from the solid. The liquor is evaporated to dryness with a rotovap. The solid brown paste obtained is treated successively with methanol to obtain a white powder which is isolated by filtration, thoroughly washed with water and methanol, and dried. The resulting Hexakis(4-benzyloxyphenoxy)cyclotriphosphazene trimer is purified by multiple crystallizations from 50% THF/CH3OH mixtures.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06093758 |
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| Source dataset | uspto-grants-2000_07 |
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| ORD ID | ord-c877a5f667fd41b6aca817b0d4c7df74 |
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| Source note | uspto-grants-2000_07 |
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