Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| Edukt | (3-Cyanophenyl-hydroxy-methyl]-phosphonic acid dimethyl ester | HCID 86654332 | — |
| Katalysator | p-Toluenesulfonic acid | HCID 6101 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | HCID 86654333 | HCID 86654333 | 100% |
Reaktionsschritte
3,4-Dihydro-2H-pyran (10.83 g, 128.70 mmol) and p-toluenesulfonic acid (0.34 g, 1.75 mmol) were added to a solution of [(3-cyanophenyl-hydroxy-methyl]-phosphonic acid dimethyl ester (14.10 g, 58.50 mmol) in dry toluene (195 ml) and the reaction mixture was stirred under nitrogen atmosphere at 50° C. for 3 h. The solvent was then removed under vacuum and the residue was taken up with ethyl acetate (100 ml). The organic layer was washed with a saturated NaHCO3 solution (1×100 ml), brine (1×100 ml) and dried over Na2SO4. The filtrate was evaporated to dryness to give the crude [(3-cyano-phenyl)-(tetrahydro-pyran-2-yloxy)-methyl]phosphonic acid dimethyl ester as a yellow oil (19 g, 58.46 mmol, 100%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08946250B2 |
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| Quelldatensatz | uspto-grants-2015_02 |
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| ORD ID | ord-3d2c6ebac3a7411eb47c180529aec035 |
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| Quellennotiz | uspto-grants-2015_02 |
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