Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 59073804 | HCID 59073804 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59073689 | HCID 59073689 | — |
Reaction Steps
To a solution of the crude azide (500 mg, 3.03 mmol) in THF (15 mL) were added Ph3P (polymer-supported, 3.0 mmol/g, 1.5 eq.) and water (5 mL). The reaction mixture was stirred at 60° C. until reaction completion, cooled down to rt and filtered. Sat. aq. NaHCO3 and EA were then added, the layers separated and the aq. layer extracted with EA (1×). The combined organic extracts were dried over Na2SO4, filtered and concentrated under reduced pressure. The crude residue was purified by FC (9:1 CH2Cl2/MeOH) and the title compound was obtained as an orange oil. LC-MS-conditions 02: tR=0.27 min; [M+AcCN+H]+=181.61.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08563714B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-945379cb4b884cc691a99278c2e6bc4e |
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| Source note | uspto-grants-2013_10 |
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