Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Benzyl Bromide | HCID 7498 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 1H-Purine-2,6-dione, 3,7-dihydro-3-butyl- | HCID 218667 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 7-Benzyl-3-butylxanthine | HCID 3993866 | — |
Reaktionsschritte
10 g (0.25 mol) of sodium hydroxide dissolved in 100 ml of water were added to a suspension of 52 g (0.25 mol) of 3-butylxanthine in 300 ml of methanol and the reaction mixture was stirred at 70° C. for one hour, then treated dropwise at the same temperature with 42.8 g (0.25 mol) of benzyl bromide and kept between 70° and 80° C. for 5 hours. 1.0 g (0.025 mol) of sodium hydroxide and 4.28 g (0.025 mol) of benzyl bromide were then added. After a further 2 hours, the mixture was cooled, diluted with 1500 ml of water and filtered cold on a suction filter, the product was washed with water on the suction filter and dissolved in 1000 ml of 1 N sodium hydroxide solution, and the solution was filtered and slowly brought to pH 3 with stirring using concentrated hydrochloric acid. The crystallizate was filtered off from the solution, washed with water until chloride-free and dried under reduced pressure.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06214992B1 |
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| Quelldatensatz | uspto-grants-2001_04 |
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| ORD ID | ord-be0c83a3a4894dbaba00268796799358 |
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| Quellennotiz | uspto-grants-2001_04 |
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