Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 135410979 | HCID 135410979 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 135410980 | HCID 135410980 | 88% |
Reaction Steps
A solution of the product of Example 454 (25.5 mg, 0.389 mmol) in 1 mL of 1N aqueous sodium hydroxide and 1ML of methanol was stirred at 25° C. for 17 hours, and concentrated under a stream of warm nitrogen. The residue was treated with 2 mL of 1N aqueous hydrochloric acid. The resulting solid was isolated by vacuum filtration, washed with 10 mL of water, and dried to provide the title compound (21.4 mg, 88% yield). 1H NMR (300 MHz, DMSO-d6) δ 0.98 (d, J=6.62 Hz, 6 H) 1.56 (m, 2 H) 1.68 (m, 1 H) 4.48 (m, 2 H) 7.32-7.53 (m, 4 H) 7.59 (m, 2 H) 7.69 (d, J=8.82 Hz, 1 H) 7.75 (s, 1 H) 8.55 (dd, J=8.09, 1.84 Hz, 1 H) 8.88 (dd, J=4.78, 1.47 Hz, 1 H) 10.79 (s, 1 H) 10.88 (s, 1 H) 13.01 (bs, 1 H) 14.12 (bs, 1 H). MS (ESI+) m/z 627.1 (M+H)+, 649.1 (M+Na)+, (ESI−) m/z 625.1 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07902203B2 |
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| Source dataset | uspto-grants-2011_03 |
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| ORD ID | ord-6f5e457521884f7493dd1d2bc8be8411 |
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| Source note | uspto-grants-2011_03 |
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