HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 10710411, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-(Bromomethyl)-1,3-difluorobenzene | HCID 581435 | — |
| Reactant | 2,6-Dichloropurine | HCID 5324412 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 10710411 | HCID 10710411 | 61% |
Reaction Steps
To a stirred solution of 2,6-dichloropurine (5.3 mmol) in 10 ml anhydrous DMSO at room temperature was added anhydrous potassium carbonate (6.34 mmol) and 2,6-difluorobenzylbromide (6.34 mmol). The reaction mixture was maintained at this temperature for 20 hrs. The reaction can be monitored using either TLC or LC/MS. The reaction mixture was poured in to a beaker containing ice-cold water. The aqueous layer was acidified to pH 5-6. Extraction of the aqueous layer, using 3×75 ml portions of ethyl acetate, afforded the crude product. This was purified on the silica gel column (10-70% ethyl acetate in petroleum ether, step-gradient), to give the desired compound in a yield of 61%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247410B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-10d396c0a6b24c75a35d729c1fd4b8a6 |
| Source note | uspto-grants-2012_08 |