Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 11742215 | HCID 11742215 | — |
| Product | HCID 58659454 | HCID 58659454 | — |
Reaction Steps
1-[4-(6-Chloro-pyrimidin-4-yloxy)-phenyl]-3-(3-trifluoromethyl-phenyl)-urea (Example 56) (42.7 mg, 0.1 mmol) is dissolved in methylamine (30% in EtOH, 1 mL) in a sealable tube and heated under Ar for 10 min at 50° C. After evaporating the solvent, the product is purified by preparative TLC (2 20×20 cm plates, acetone/CH2Cl2=3:7) to give the title compound as a white solid: M+H=404.1; 1H-NMR (400 MHz, CDCl3): 8.22 (s, 1H, pyridinyl), 7.84 (s/broad, 1H, NH), 7.62 (s, 1H, 3-CF3-phenyl), 7.52 (d, 8.0 Hz, 1H, CF3-phenyl), 7.35 (t, 8.0 Hz, 1H, 3-CF3-phenyl), 7.28 (m, 3H, CF3-phenyl/oxo-phenyl-amine), 6.97 (d, 9.5 Hz, 2H, oxo-phenyl-amine), 5.62 (d/broad, 2H, pyridinyl), 5.44 (s/broad, 1H, NH), 2.89 (s/broad, CH3—N); Rf (acetone/CH2Cl2=3:7): 0.36.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07652022B2 |
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| Source dataset | uspto-grants-2010_01 |
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| ORD ID | ord-289728be034b4abc8cf72c70a3d12bb0 |
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| Source note | uspto-grants-2010_01 |
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