Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | P-Anisidine | HCID 7732 | — |
| Reactant | HCID 178491934 | HCID 178491934 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 178492151 | HCID 178492151 | — |
Reaction Steps
A mixture of 1-[trans-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-7-chloro-3-(4-methoxy-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one (0.20 g, 0.40 mmol) (from Example 19a supra) and p-anisidine (63.6 mg, 0.52 mmol) (Aldrich) in 2-propanol (4 mL) was placed in a microwave reactor (SmithSynthesizer™). The reaction mixture was heated at 160° C. for 10 minutes. After cooling, it was concentrated under reduced pressure. The residue was purified by flash chromatography eluting with ethyl acetate-hexanes (3:7 then 2:3) to give 1-[trans-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-3-(4-methoxy-phenyl)-7-(4-methoxy-phenylamino)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one. (Yield 0.14 g, 58%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07115740B2 |
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| Source dataset | uspto-grants-2006_10 |
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| ORD ID | ord-760334091dad4ed1bd061e6397b0a116 |
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| Source note | uspto-grants-2006_10 |
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