Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | p-Chlorophenethylic alcohol | HCID 74647 | — |
| Edukt | Diethyl azodicarboxylate | HCID 5462977 | — |
| Edukt | Methyl 4-chloro-3-hydroxybenzoate | HCID 11819787 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 69652314 | HCID 69652314 | — |
Reaktionsschritte
g (5.36 mmol) of 4-Chloro-3-hydroxy-benzoic acid methyl ester was dissolved in 40 ml of anhydrous tetrahydrofuran. To this solution was added 0.923 g (5.9 mmol) of 2-(4-chloro-phenyl)-ethanol, 5.35 g (equivalent to 16.1 mmol PPh3) of triphenylphosphine derivatized polystyrene and 2.80 g (16.1 mmol) of DEAD. The solution was shaken for 16 h at RT. The polymer was filtered off and washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was taken-up in ethyl acetate and the solution was washed three times with water and twice with saturated aqueous sodium chloride. The organic phase was dried with magnesium sulphate, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel eluting with ethyl acetate/n-heptane (1/5). Yield 1.6 g. LC-MS (ES+): m/e=325 (M)+
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06953857B2 |
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| Quelldatensatz | uspto-grants-2005_10 |
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| ORD ID | ord-9197bb0f980240dcb069db6298e7d5f0 |
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| Quellennotiz | uspto-grants-2005_10 |
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