Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Borane;tetrahydrofuran | HCID 2723981 | — |
| Edukt | (2R)-6-Iodochromane-2-carboxylic acid | HCID 9966213 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | [(2R)-6-iodo-3,4-dihydro-2H-chromen-2-yl]methanol | HCID 9943850 | — |
Reaktionsschritte
To a solution of (2R)-6-iodo-3,4-dihydro-2H-chromene-2-carboxylic acid (Example 7, 19.5 mmol, 1.0 eq.) in THF (45 mL) at 10° C. was added dropwise a solution of borane-THF complex (1M in THF, 23.4 mmol, 1.2 eq). The resulting reaction mixture was stirred at 45° C. for 1.5 hours and was then cooled to 10° C. Next, water was added followed by saturated NaHCO3 solution. The resulting two-phase mixture was separated and the aqueous phase was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, concentrated to afford the product as a white solid in quantitative yield that was used without further purification. GC-MS m/z 290 (M+)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06919371B2 |
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| Quelldatensatz | uspto-grants-2005_07 |
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| ORD ID | ord-d408dc4064424a799a8277a775e39f72 |
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| Quellennotiz | uspto-grants-2005_07 |
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