HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 136230085, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 136377276 | HCID 136377276 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 136230085 | HCID 136230085 | 15.5% |
Reaction Steps
400 mg (0.59 mmol) of impure 2-amino-7-(3-chloro-4-hydroxy-phenyl)-1-ethyl-3-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-imidazol-2-yl]-1H-[1,8]naphthyridin-4-one was dissolved in 20 ml DCM. At 0° C., 3.39 g of TFA were added and the mixture was stirred at room temperature for 24 hours. The solution is neutralized by adding an excess of aqueous NaHCO3 solution. The mixture was then extracted three times with DCM. The combined organic phases were dried over MgSO4 and the solvents were evaporated off under reduced pressure. The so-gained raw material was purified on silica gel (DCM:MeOH:NH4OH=4:10.1) yielding 0.035 g of the unprotected title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126972B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-81f3240c0dcb475f8511bf04fb8c89bf |
| Source note | uspto-grants-2015_09 |