HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetate → HCID 66776742, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetate | HCID 175 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Pyrosulfite | HCID 656671 | — |
| Reactant | HCID 66777001 | HCID 66777001 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66776742 | HCID 66776742 | — |
Reaction Steps
Bromine (3.6 ml, 70.4 mmol) was added dropwise, at −14° C., to 1-(6-amino-9-methyl-9H-purin-2-yl)butan-1-ol (1700 mg, 7.69 mmol) dissolved in a mixture of MeOH (20 ml), THF (20 ml) and acetate buffer pH 4 (20 ml) (obtained by dissolving 4 g of sodium acetate in 100 ml of water and by adjusting pH 4 with glacial acetic acid). The reaction was stirred at this temperature for 15 minutes and then at RT for 10 minutes. Excess of bromine was eliminated with sodium metabisulphite and the reaction brought to pH 8 by addition of saturated solution of Na2CO3. The organic solvents were evaporated under reduced pressure, to give a solid that was filtered and used for the following reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133197B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-03d5781878d1409fa910bdc3310bb056 |
| Source note | uspto-grants-2015_09 |