Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Salbutamol | HCID 2083 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Glycodeoxycholic Acid | HCID 3035026 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 131722754 | HCID 131722754 | 105,9% |
Reaktionsschritte
Salbutamol base (1.2007 g; 5.02 mmol) was dissolved in ethanol (100 mL) with vigorous stirring. Glycodeoxycholic acid (2.4601 g; water content: 4.25% w/w; 5.25 mmol˜5% molar excess) was added and dissolved with stirring. A clear, colourless solution was obtained. The ethanol was removed by vacuum rotary-evaporation to give a viscous, yellow residue. Ethyl acetate (200 mL) was added to the residue and the mixture heated in a water bath with constant agitation. As the yellow residue dissolved, a white precipitate formed. Agitation was continued until the yellow residue disappeared. The ethyl acetate solution was cooled in an ice bath. The precipitate was isolated by vacuum filtration and dried in a vacuum oven at 40° C. for 20 hours to give salbutamol glycodeoxycholate (3.662 g; water content; 4.95% w/w; % yield; 97.9%). Analysis by differential scanning calorimetry from 50 to 200° C. gave no significant thermal event. Slow decomposition was evident after 110° C. A saturated aqueous solution gave a pH of 6.12. The aqueous solubility was greater than 8.35 mg/mL. The theoretical percentage of salbutamol base in the salbutamol glycodeoxycholate 34.74%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06255502B1 |
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| Quelldatensatz | uspto-grants-2001_07 |
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| ORD ID | ord-2df3eac4f00b4382adc03e49033db230 |
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| Quellennotiz | uspto-grants-2001_07 |
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