Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Formic Acid | HCID 284 | — |
| Edukt | Acetic Anhydride | HCID 7918 | — |
| Edukt | o-Aminophenethyl alcohol | HCID 79282 | — |
| Edukt | Potassium Bicarbonate | HCID 516893 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 21088387 | HCID 21088387 | — |
Reaktionsschritte
12.6 ml of formic acid were added dropwise at 0° C. to 15 ml of acetic anhydride, and the mixture was then stirred for 2 hours at 60° C. After cooling to 20° C., the mixture was diluted with 140 ml of tetrahydrofuran, cooled to −4° C., and at this temperature a solution of 18.4 g of 2-(2-aminophenyl)ethanol in 185 ml of tetrahydrofuran was added dropwise. After stirring for 3 hours at −6° C. the mixture was neutralised with aqueous potassium hydrogen carbonate solution (25% KHCO3) and extracted four times with 300 ml of ethyl acetate each time. The combined extracts were dried over sodium sulfate and concentrated by evaporation in vacuo. 18.4 g (94% of theory) of the title compound were thereby obtained in the form of yellowish crystals that melted at 49–54° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07183274B2 |
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| Quelldatensatz | uspto-grants-2007_02 |
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| ORD ID | ord-51ee964ad2ee4f0bb2b2ff761a5b33c9 |
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| Quellennotiz | uspto-grants-2007_02 |
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