Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethyl phosphonoacetate | HCID 13345 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 91618982 | HCID 91618982 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131733920 | HCID 131733920 | — |
Reaction Steps
Under a nitrogen atmosphere, to a suspension of 60% sodium hydride (2.76 g) in THF (100 mL) was added ethyl diethylphosphonoacetate (15.2 mL) at 0° C., and the mixture was stirred at 0° C. for 5 min. To the obtained colorless solution was added cyclopropyl(5-fluoro-2-methoxypyridin-4-yl)methanone (entire amount) obtained in Example 42, step B, at 0° C., and the mixture was stirred at room temperature for 30 min. To the reaction mixture was added water at room temperature, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give a crude product of the title compound as a brown oil. This compound was used for the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09181186B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-a96ed7e7396c475ab0b850e8fc6c7689 |
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| Source note | uspto-grants-2015_11 |
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