Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 3-Hydroxy-2-naphthoic acid | HCID 7104 | — |
| Edukt | Imipramine Hydrochloride | HCID 8228 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | Imipramine | HCID 3696 | 105,5% |
Reaktionsschritte
To a solution containing 7.7 g of 3-hydroxy-2-napthoic acid in 75.0 g of USP water was added as necessary dilute HCl or NaOH solution to adjust the solution to about pH 9.4. To a second solution of 13.6 g of imipramine HCl in 100.0 g of USP water was added as necessary dilute HCl or NaOH solution to adjust the solution to about pH 4.5. The imipramine HCl solution was added to the 3-hydroxy-2-napthoic sodium salt solution over a period of about 2 h. The mixture was stirred and held at around 50° C. for at least 18 h. The mixture was cooled to below 25° C. and the solids were collected by filtration. The solid cake was washed with USP water (2×100 g). The solid cake was dried at 105° C. under vacuum to yield a powder (12.7 g) and characterized by DSC (FIG. 13), FTIR (FIG. 14) and 1H NMR (FIG. 15).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08575151B1 |
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| Quelldatensatz | uspto-grants-2013_11 |
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| ORD ID | ord-eb117042276d4c53b2828c1c64e41330 |
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| Quellennotiz | uspto-grants-2013_11 |
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