Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 178476761 | HCID 178476761 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178503031 | HCID 178503031 | — |
Reaction Steps
A solution of 26-f (0.98 g, 2.03 mmol) in 15 ml of dioxane was treated with 2 ml of 5N NaOH and heated at 80° C. for 2 hour. The reaction solution was cooled to room temperature and then concentrated under vacuum and the residue was diluted with water and washed with ethyl acetate. The aqueous layer was acidified with conc. HCl to pH=1 and the resulting solids were collected via filtration to give 26-1 (170 mg 38.4%). 1H NMR (300 MHz, DMSO-d6): δ 10.06 (s, 1H), 8.60 (s, 1H), 8.37 (s, 1H), 8.04 (s, 1H), 7.70 (m, 2H), 7.50 (m, 2H), 6.70 (s, 1H), 4.87 (m, 1H), 1.52 (m, 9H), 1.15 (m, 5H). (M+H)+=456.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09079930B2 |
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| Source dataset | uspto-grants-2015_07 |
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| ORD ID | ord-0cf65df1e6a14d109e56f08cb00a9c4c |
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| Source note | uspto-grants-2015_07 |
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