Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 4-(4-Nitronaphthalen-1-yloxy)pyridin-2-amine | HCID 58532562 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67238714 | HCID 67238714 | — |
Reaction Steps
To a solution of 4-(4-nitronaphthalen-1-yloxy)pyridin-2-amine (100 mg, 0.356 mmol) and Et3N (100 μL, 0.71 mmol) in dry THF was added phenyl carbonochloridate (49 μL, 0.39 mmol) and the mixture maintained at RT for 2 hr. Pyrrolidine (88 μL, 1.068 mmol) was added and after 16 h at RT the resulting mixture was partitioned between aq NH4Cl (10 mL) and DCM (10 mL). The aq layer was separated and extracted with DCM (3×10 mL) and the combined organic extracts were dried (MgSO4) and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, 40 g, EtOAc in isohexane, 0-100%, gradient elution) to afford N-(4-(4-nitronaphthalen-1-yloxy)pyridin-2-yl)pyrrolidine-1-carboxamide, Intermediate K2, as a yellow solid (110 mg, 79%); Rt 1.84 min (Method 2); m/z 379 (M+H)+ (ES+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08299074B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-b18cac1654fc4e5b80a6968d24eb62f0 |
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| Source note | uspto-grants-2012_10 |
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