HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-Amino-2-{[2-(ethyloxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-(2-ethoxyethoxy)-8-methoxy-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purin-6-amine | HCID 57699730 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 6-Amino-2-{[2-(ethyloxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one | HCID 57699708 | — |
Reaction Steps
To a solution of 2-(2-ethoxyethoxy)-8-methoxy-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purin-6-amine (245 mg) in dry methanol (10 ml) at room temperature and under nitrogen was added 4.0M hydrogen chloride in 1,4-dioxane (4.0 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 (90 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977344B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-341d3d07536d428aaffa0398c1a950cc |
| Source note | uspto-grants-2011_07 |