HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetate → HCID 66671727, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetate | HCID 175 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 66671498 | HCID 66671498 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 66671727 | HCID 66671727 | — |
Reaction Steps
Bromine (0.89 ml, 17.5 mmol) was added dropwise at 0° C. to a solution of dibenzyl-{9-methyl-2-[2-(2,5,5-trimethyl-[1,3]dioxan-2-yl)-ethyl]-9H-purin-6-yl}-amine (1.7 g, 3.50 mmol) in 20 ml of a mixture of MeOH/THF (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 RT for two hours. 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 in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133197B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-9ca93fa66ae0495ab8855d14b1fa6e08 |
| Source note | uspto-grants-2015_09 |