Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Fluoro-1-methyl-3-nitrobenzene | HCID 13470957 | — |
| Reactant | HCID 86713567 | HCID 86713567 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86713568 | HCID 86713568 | 52.3% |
Reaction Steps
To a solution of 6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-2-amine (400 mg, 1.42 mmol) in THF (20 mL) at 0° C. was added sodium hydride (102 mg, 4.25 mmol). The solution was stirred for 20 mins, followed by the addition of 2-fluoro-1-methyl-3-nitrobenzene (440 mg, 2.84 mmol). The reaction mixture was stirred at RT overnight, quenched by water (20 mL) and extracted with ethyl acetate (3×30 mL). The organic layers were combined, washed with brine (50 mL), dried over sodium sulfate, filtered, and concentrated to afford a crude product, which was purified by silica gel column chromatography (ethyl acetate:petroleum ether=4:1) to afford 6-(3,5-dimethoxyphenyl)-N-(2-methyl-6-nitrophenyl)pyrido[2,3-d]pyrimidin-2-amine (310 mg, 51%) as a brown solid. MS (ES+) C22H19N5O4 requires: 417. found: 418 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09340514B2 |
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| Source dataset | uspto-grants-2016_05 |
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| ORD ID | ord-878a1b6ce6e043f49bb9465c784a82ed |
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| Source note | uspto-grants-2016_05 |
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