Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Oxolane--water (1/1) | HCID 21881883 | — |
| Reactant | HCID 57517487 | HCID 57517487 | — |
| Product | HCID 57517488 | HCID 57517488 | — |
Reaction Steps
A solution of 3-(2-azidopropoxy)-1-(diphenylmethyl)azetidine (350 mg) and triphenylphosphine (340 mg) in THF/water (15 mL/5 mL) was heated under reflux for 2 hr. The mixture was allowed to cool, 1M hydrochloric acid was added thereto, and the mixture was washed with diethyl ether. The obtained aqueous solution was neutralized with saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The obtained organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was dissolved in ethyl acetate (15 mL), acetic anhydride (1 mL) was added thereto, and the mixture was stirred at 60° C. for 5 hr. The mixture was allowed to cool, washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give the title compound (0.31 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08703758B2 |
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| Source dataset | uspto-grants-2014_04 |
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| ORD ID | ord-1766e566a6154ade897845d96b2bb02d |
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| Source note | uspto-grants-2014_04 |
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