Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sucrose | HCID 5988 | — |
| Edukt | Methyl 4-hydroxy-5,6-dihydro-2H-thiopyran-3-carboxylate | HCID 67482118 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 11105894 | HCID 11105894 | 99,3% |
Reaktionsschritte
A suspension of baker's yeast (Saf-Instant yeast, 30 g) in water (700 mL) was treated with sucrose (142 g). The mixture was stirred at 25° C. for 6 h. At this time, 4-hydroxy-5,6-dihydro-2H-thiopyran-3-carboxylic acid methyl ester (4.06 g, 23.31 mmol) was added. The resulting slurry was stirred at 25° C. for 22 h and then was filtered through a pad of celite. The filtrate was extracted with ethyl acetate (5×300 mL). The combined organic extracts were washed with a saturated aqueous sodium chloride solution (1×150 mL), dried over magnesium sulfate, filtered, and concentrated in vacuo. Biotage chromatography (FLASH 40M, Silica, 3/1 hexanes/ethyl acetate) afforded 4(S)-hydroxy-tetrahydro-thiopyran-3(R)-carboxylic acid methyl ester (4.08 g, 99.3%) as a colorless oil: [α]23589=+37.76° (c=2.9, methanol)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07105671B2 |
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| Quelldatensatz | uspto-grants-2006_09 |
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| ORD ID | ord-d9b08e78355b4509a0c96d5940b1d659 |
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| Quellennotiz | uspto-grants-2006_09 |
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