HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 178461594, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | HCID 178461598 | HCID 178461598 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178461594 | HCID 178461594 | 53.1% |
Reaction Steps
2,6-Bis-((R)-3-methyl-morpholin-4-yl)-9H-purine (637 mg, 2 mmol) was dissolved in 50 mL of CH2Cl2 and stirred under argon. Bromine (124 μl, 2.4 mmol) was dissolved in 2 mL of CH2Cl2 and added within 2 minutes. The reaction was stirred for 6 hours at room temperature. 5 mL of aqueous Na2S2O3 were added, the mixture was stirred for 15 minutes, and the organic solvents were separated, washed with brine and aqueous NaHCO3, dried over Na2SO4, filtered, and concentrated. The residue was purified by column chromatography (40 g SiO2, heptane/EtOAc in a gradient from 2/3 to 4/1) to give a foam (422 mg, 53%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09334271B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-319576340b954a64976ccafcf3097766 |
| Source note | uspto-grants-2016_05 |