HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 66777068, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 66671496 | HCID 66671496 | — |
| Solvent | Acetate | HCID 175 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 66777068 | HCID 66777068 | — |
Reaction Steps
Bromine (2.1 ml, 41 mmol) was added dropwise at −14° C. to a solution of 4-(6-amino-9-methyl-9H-purin-2-yl)butan-2-ol (800 mg, 3.60 mmol) in a mixture of MeOH/THF (20 ml, 1/1) and acetate buffer pH=4 (10 ml). The latter was obtained dissolving 4 g of sodium acetate in 100 ml of water and by adjusting to pH 4 through addition of glacial acetic acid. The reaction was stirred at this temperature for 10 minutes and then at RT for 10 minutes. Excess of bromine was quenched by addition of sodium metabisulphite and the reaction was brought to pH 8 by addition of a saturated solution of Na2CO3. The organic solvents were evaporated under reduced pressure, to give a solid that was filtered and used without any further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133197B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-815e9891252a4583be99151e67c693d7 |
| Source note | uspto-grants-2015_09 |