Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 178476760 | HCID 178476760 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178503030 | HCID 178503030 | — |
Reaction Steps
A solution of 27-e (0.90 g, 1.86 mmol) in 30 ml of dioxane was treated with 3 ml of 3N NaOH and heated at 80° C. for 2 hour. The mixture 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 resulting solids were collected via filtration to give 27-1 (400 mg 47.2%). 1H NMR (300 MHz, DMSO-d6): δ 10.06 (br, 1H), 8.62 (s, 1H), 8.38 (s, 1H), 8.07 (s, 1H), 7.70 (m, 2H), 7.39 (m, 2H), 6.73 (s, 1H), 4.88 (m, 1H), 1.52 (m, 9H), 1.16 (m, 5H). (M+H)+=456.2.
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-6a1ffd8fcffd48dcb8707b0397ce5282 |
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| Source note | uspto-grants-2015_07 |
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