Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Pyridinecarboxaldehyde | HCID 14273 | — |
| Reactant | Tetraethyl methylenediphosphonate | HCID 15455 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59750189 | HCID 59750189 | 94% |
Reaction Steps
A solution of tetraethyl methylenediphosphonate (3.7 g, 13 mmol) in tetrahydrofuran (5 ml) was added dropwise to a mixture of sodium hydride (60% in oil, 750 mg, 18 mmol) and tetrahydrofuran (15 ml) at 0° C., and the mixture was stirred at the same temperature for 20 minutes. Successively, a solution of 2-pyridinecarbaldehyde (1.3 g, 12 mmol) in tetrahydrofuran (5 ml) was added dropwise to the mixture at 0° C., and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was combined with water and extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with ethyl acetate-methanol (20:1, v/v) were collected and concentrated to give the titled compound (2.7 g, 94%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07767665B2 |
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| Source dataset | uspto-grants-2010_08 |
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| ORD ID | ord-fafa0f17512c46b5995b7bc3dfeb3a06 |
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| Source note | uspto-grants-2010_08 |
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