HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 6-Amino-2-{[1-methyl-2-(methoxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 2-{[1-Methyl-2-(methyloxy)ethyl]oxy}-8-(methoxy)-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purin-6-amine | HCID 57699698 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 6-Amino-2-{[1-methyl-2-(methoxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one | HCID 57699660 | — |
Reaktionsschritte
To a solution of 2-{[1-methyl-2-(methoxy)ethyl]oxy}-8-(methyloxy)-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purin-6-amine (290 mg) in dry methanol (12 ml) at room temperature and under nitrogen was added 4.0M hydrogen chloride in 1,4-dioxane (5.0 ml). The reaction was left to stir at room temperature for 1 hour. The reaction was concentrated in vacuo and the resulting residue purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (10-45%) to afford a white solid. This was taken up in water (15 ml) and neutralised by the addition of 2.0M sodium hydroxide solution. The solid was filtered and dried on the rotary evaporator (60° C.) for 30 minutes (50 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07977344B2 |
| Quelldatensatz | uspto-grants-2011_07 |
| ORD ID | ord-bcdbcec334684310b0c09c1ec7eae64b |
| Quellennotiz | uspto-grants-2011_07 |