Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Methoxyethanol | HCID 8019 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86685395 | HCID 86685395 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68015333 | HCID 68015333 | — |
Reaction Steps
To a solution of 2-methoxyethanol (0.019 ml) in N,N-dimethylformamide (3 ml) was added sodium hydride (60% in oil, 9 mg) at room temperature, and the mixture was stirred for 30 min. 8-Chloro-2-ethoxy-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[3,4-d]pyrimidin-4(3H)-one (80 mg) was added to reaction mixture, and the mixture was stirred at 60° C., for 5 hr, and allowed to be cooled to room temperature. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane). The obtained residue was suspended in a mixed solvent of ethyl acetate/hexane, and the resulting solid was collected by filtration to give the title compound (21 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09023858B2 |
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| Source dataset | uspto-grants-2015_05 |
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| ORD ID | ord-072f25e5d2444299919617b240d29dd3 |
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| Source note | uspto-grants-2015_05 |
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