Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 22136183 | HCID 22136183 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10108875 | HCID 10108875 | — |
Reaction Steps
A mixture of the product from part 9 (95 mg), BOP (220 mg), piperidine (56 mg) and TEA (67 mg) in 2 ml of DMF is stirred at room temperature for 18 hours. The mixture is added to aqueous NaHCO3 solution and extracted with EtOAc. The organic layer is washed with brine and water, dried (Na2SO4), filtered and concentrated to afford a foam. Purification on a silica gel column, eluting with 5% methanol in methylene chloride, gives the title compound. 1H NMR (CDCl3) δ 1.38-1.50 and 1.60-1.80 (6H, m), 3.18-3.36 (2H, m), 3.65-3.95 (2H, m), 7.40-7.60 (6H, m), 7.75 (2H, d), 7.95 (1H, s), 8.05 (1H, s), 8.10 (1H, d). The hydrochloride salt was prepared by treating the free base in EtOAc with a solution of hydrogen chloride in ether and collecting by filtration.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06511987B1 |
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| Source dataset | uspto-grants-2003_01 |
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| ORD ID | ord-919e7cc1469b462195e35456f3277ac1 |
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| Source note | uspto-grants-2003_01 |
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