Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Alprazolam | HCID 2118 | — |
| Edukt | p-Toluenesulfonic acid | HCID 6101 | — |
| Edukt | Acetyl chloride | HCID 6367 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Dimethylmethyleneammonium chloride | HCID 21939857 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | U 43465F | HCID 134388 | — |
Reaktionsschritte
The resulting solid, dimethylmethyleneammonium chloride, was suspended in tetrahydrofuran, cooled in an ice bath, treated with 8-chloro-1-methyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine (3.09 g., 0.01 mole; and then dropwise with acetyl chloride (0.07 ml., 0.001 mole). This mixture was kept in the ice bath for 3 hours, poured into ice cold, dilute sodium bicarbonate and extracted with methylene chloride. The extract was washed with a dilute salt solution, dried over anhydrous sodium sulfate and concentrated in vacuo. A solution of the residual oil in ethanol was treated with a solution of 1 equivalent of p-toluenesulfonic acid in ethanol and the 8-chloro-1-[2-(dimethylamino)ethyl]-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine p-toluenesulfonate was isolated by crystallization.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04075221 |
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| Quelldatensatz | uspto-grants-1978_02 |
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| ORD ID | ord-855f2e2c6e30481fb1eae77ff27d68fe |
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| Quellennotiz | uspto-grants-1978_02 |
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