Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Pyrosulfite | HCID 656671 | — |
| Reactant | HCID 66671682 | HCID 66671682 | — |
| Solvent | Acetate | HCID 175 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66671626 | HCID 66671626 | — |
Reaction Steps
Bromine (0.4 ml, 6.8 mmol) was added dropwise, at −14° C., to 4-(6-amino-9-methyl-9H-purin-2-yl)butan-1-ol (250 mg, 1.13 mmol) dissolved in a mixture of dioxane (5 ml) and acetate buffer pH 4 (2.5 ml) (obtained by dissolving 4 g of sodium acetate in 100 ml of water and by adjusting to pH 4 with glacial acetic acid). The reaction was stirred at this temperature for 10 minutes and then at RT for 15 minutes. Excess of bromine was eliminated with sodium metabisulphite and the reaction brought to pH 8 by addition of saturated solution of Na2CO3. The aqueous phase was extracted with DCM (6×10). The organic phases were dried over anhydrous sodium sulphate and evaporated under reduced pressure, to give a residue that was used for the following reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09133197B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-a94abd10c0fe4decbc4678d2d5447dbe |
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| Source note | uspto-grants-2015_09 |
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