Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 91233241 | HCID 91233241 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66820044 | HCID 66820044 | — |
Reaction Steps
To a solution of the crude azide (565 mg, 2.50 mmol) in THF (12 mL) were added polymer-supported Ph3P (2.0 eq.) and water (4 mL). The reaction mixture was stirred at 60° C. until completion of the reaction, cooled down to rt, filtered and partitioned between EA and sat. aq. NaHCO3. The layers were separated and the aq. layer extracted with EA. The combined org. extracts were dried over MgSO4, filtered and concentrated under reduced pressure to give the title compound as a brown oil after purification by FC (CH2Cl2-MeOH 1:0 to 9:1). LC-MS-conditions 01: tR=0.38 min; [M+H]+=200.96.
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-b62c72f7811948ad9db581cd9c16fbb4 |
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| Source note | uspto-grants-2013_10 |
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