Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Selectfluor | HCID 2724933 | — |
| Reactant | HCID 67066357 | HCID 67066357 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67066280 | HCID 67066280 | 29% |
Reaction Steps
The fluorination procedure was performed as described in Lal, G S, et al. J. Org. Chem., 60:7340-7342 (1995). The product from Example 41A, Part B (0.42 g, 1.26 mmol) and Selectfluor™ (0.672 g, 1.9 mmol) were combined in a mixture of acetonitrile (8 mL) and methanol (1 mL) and heated at 90° C. under N2 for 5 h. The solution was diluted with water, extracted into ethyl acetate, washed with sodium bicarbonate solution, concentrated and purified by column chromatography on silica gel to give the title compound (0.138 g, 29%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09095590B2 |
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| Source dataset | uspto-grants-2015_08 |
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| ORD ID | ord-7f0f16cacdd847f28f884105bd53479a |
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| Source note | uspto-grants-2015_08 |
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