Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Lithium iodide | HCID 66321 | — |
| Reactant | HCID 68863619 | HCID 68863619 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 68866375 | HCID 68866375 | 22.3% |
Reaction Steps
A mixture of Example 487A (0.064 g, 0.14 mmol) in 1.4 mL pyridine was treated with LiI (0.068 g, 0.5 mmol), heated to 150° C. for 25 minutes in a microwave reactor, and concentrated. The concentrate was purified by C18 reverse-phase HPLC using acetonitrile/water/0.1% TFA to provide the desired product (14.3 mg). MS (ESI(+)) m/e 458 (M+H)+; (ESI(−)) m/e 456 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.58 (dd, 1H), 7.37 (dt, 1H), 7.19 (d, 1H), 6.85 (d, 1H), 6.82 (d, 1H), 6.57 (t, 1H), 6.43 (m, 1H), 3.19 (m, 4H), 2.90 (s, 3H), 2.72, (m, 2H), 2.68 (m, 4H), 1.83 (m, 3H), 1.68 (m, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07491718B2 |
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| Source dataset | uspto-grants-2009_02 |
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| ORD ID | ord-759aaadfdbd041c8acfe76ffc99cfb19 |
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| Source note | uspto-grants-2009_02 |
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