Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Magnesium 2-(dioxidan-2-ide-1-carbonyl)benzoate--water (1/1/6) | HCID 21894687 | — |
| Reactant | HCID 22050205 | HCID 22050205 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22050060 | HCID 22050060 | 90% |
Reaction Steps
A suspension of 3-bromo-4-[(2,4-difluorobenzyl)oxy]-6-methyl-1-{[2-(methylthio)pyrimidin-4-yl]methyl}pyridin-2(1H)-one 0.28 g, 0.0006 mol), and magnesium monoperoxyphthalate hexahydrate 90.6 g, 0.0012 mol) in acetonitrile (8.0 ml) and water (2.0 ml) was stirred at room temperature for 16 h. The resulting clear solution was concentrated under reduced pressure, and the residue was partitioned between dichloromethane (30 mL) and water (20 mL). The organic phase was washed with water, dried (Na2SO4) and concentrated to afford the title compound (0.27 g, 90%) as a pale yellow substance: 1H NMR (CD3OD/400 MHz) δ 8.91 (d, 1H, J=5.2 Hz), 7.63 (d over m, 2H, J=5.2 Hz), 7.03 (m, 2H), 6.58 (s, 1H), 5.54 (s, 2H), 5.33 (s, 2H), 3.28 (s, 3H), and 2.49 (s, 3H); 19F NMR (CD3OD/400 MHz) δ−111.58 (m), −115.98 (m);ES-HRMS m/z 500.0113 (M+H C19H17N3O4BrSF2 requires 500.0086).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07067540B2 |
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| Source dataset | uspto-grants-2006_06 |
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| ORD ID | ord-19434374418149829f48104d7231b413 |
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| Source note | uspto-grants-2006_06 |
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