HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-(2,2,2-trifluoroethoxy)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-(methylsulfinyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione | HCID 86685356 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(2,2,2-trifluoroethoxy)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione | HCID 86685357 | — |
Reaction Steps
2-(Methylsulfinyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (150 mg) was suspended in tetrahydrofuran (5 ml), 2,2,2-trifluoroethanol (108 μl) was added thereto, and then sodium hydride (60% in oil, 37.6 mg) was added thereto under ice-cooling, and the mixture was stirred for 10 min. To the reaction mixture was added 0.5M hydrochloric acid (4 ml), and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained white residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (128 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09023858B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-1d6dbb20c4c74d94857bb434ac33a50d |
| Source note | uspto-grants-2015_05 |