Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Cerate(2-), hexakis(nitrato-kappaO)-, potassium (1:2), (OC-6-11)- | HCID 407333 | — |
| Reactant | HCID 11120552 | HCID 11120552 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10899575 | HCID 10899575 | 79.6% |
Reaction Steps
To a solution of (1,4-dioxaspiro[4.5]dec-7-en-8-yloxy) [tri(propan-2-yl)]silane (22.9 g) in acetonitrile (180 mL) were added dropwise sodium azide (21.4 g) and ammonium hexanitratocerate (IV) (121 g) at −20° C. The reaction mixture was stirred at −20° C. for 4 hr, ice-cooled water was added, and the mixture was extracted with diethyl ether. The extract was washed with water and saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/petroleum ether) to give the title compound (11.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08772277B2 |
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| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-b99e2f6cdde348689ac455ffcb8be3a7 |
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| Source note | uspto-grants-2014_07 |
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