Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Edukt | Methyl 3,5-dihydroxyphenylacetate | HCID 579787 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 57666065 | HCID 57666065 | — |
Reaktionsschritte
Trifluoromethanesulphonic anhydride (7.05 g, 25.0 mmol) was added dropwise to a solution of 3,5-dihydroxyphenyl acetic acid methyl ester (1.80 g, 10.0 mmol) and pyridine (4.9 mL, 60.0 mmol) in DCM (20 mL) at 0° C. The temperature was maintained at 0° C. for 15 mins before warming to room temperature and the mixture stirred for 18 hrs. The reaction was diluted with DCM washed with H2O, Na2CO3, dil. HCl, brine, dried (MgSO4) and evaporated under reduced pressure to give a yellow oil. The residue was purified by flash column chromatography (EtOAc:petroleum ether), yield 4.0 g (89%), 1H NMR (CDCl3) δ 7.31 (d, 2H), 7.17 (t, 1H), 3.74 (s, 3H), 7.73 (s, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08106236B2 |
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| Quelldatensatz | uspto-grants-2012_01 |
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| ORD ID | ord-10cdcfd1f2534856853208137ba24cd5 |
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| Quellennotiz | uspto-grants-2012_01 |
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