Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phenyl isocyanate | HCID 7672 | — |
| Reactant | HCID 21946005 | HCID 21946005 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 21946022 | HCID 21946022 | — |
Reaction Steps
(±)-[1-(2,4-Dichloro-pyrimidin-5-yl)-2-methyl-propyl]-(4-methoxy-phenyl)-amine (35.0 mg; 0.107 mmol) (from Example 11c supra) and phenyl isocyanate (12.8 μL; 0.12 mmol) (Aldrich) were combined in toluene (0.6 mL), sealed and heated in a microwave reactor (SmithCreator™, 160 seconds to a maximum of 146° C., then 800 seconds at 160° C., and finally 600 seconds at 180° C.). The reaction was incomplete, and the mixture was concentrated and purified by flash chromatography (Biotage 12M; 20:80 ethyl acetate-hexanes) to give the intermediate (±)-1-[1-(2,4-dichloro-pyrimidin-5-yl)-2-methyl-propyl]-1-(4-methoxy-phenyl)-3-phenyl-urea. (Yield 24.0 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07112676B2 |
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| Source dataset | uspto-grants-2006_09 |
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| ORD ID | ord-8728605f294e417a9f501a372388f23b |
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| Source note | uspto-grants-2006_09 |
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