HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 178461590, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | HCID 178461592 | HCID 178461592 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178461590 | HCID 178461590 | 39.8% |
Reaction Steps
To a solution of 2-chloro-6-((R)-3-methyl-morpholin-4-yl)-9H-purine (950 mg, 3.74 mmol) in CH2Cl2(19 mL) was added bromine (0.23 mL, 4.49 mmol). The mixture was stirred at ambient temperature for 19 hours. Saturated sodium thiosulfate was added. The aqueous layer was extracted with dichloromethane two times. Organic layers were combined and dried over Na2SO4 and solvent was removed under reduced pressure. The crude was purified by flash column chromatography (0-70% EtOAc/cyclohexane gradient) to furnish product as a white solid (495 mg, 39%). LC-MS at 254 nm; [M+H] 334.1; Rt 0.89 min; (LCMS method 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09334271B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-9d7b07c8173d4d5faf5ab734bd8057fa |
| Source note | uspto-grants-2016_05 |