Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 118062643 | HCID 118062643 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1773508-76-1 | HCID 118062574 | 99% |
Reaction Steps
To a stirred solution of Intermediate 317A (200 mg, 0.868 mmol) in THF (2 mL) and water (1 mL) was added NaOH (104 mg, 2.61 mmol) at RT and the reaction mixture was warmed to 50° C. and stirred for 12 h. The reaction mixture was concentrated under a reduced pressure, the residue was to pH 2 with a 1.5 N aq. solution of HCl and extracted with Et2O (3×15 mL) The combined organic layer was dried over Na2SO4, filtered and the filtrate concentrated to afford Intermediate 317B as a colorless liquid (0.12 g, 99%). 1H NMR (300 MHz, DMSO-d6) δ ppm 12.38-11.71 (m, 1H), 2.68-2.50 (m, 2H), 1.86-1.66 (m, 2H), 1.43 (s, 3H), 0.62-0.19 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09273058B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-6e4745c9c5bb4814ae456e5acc0a6425 |
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| Source note | uspto-grants-2016_03 |
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