HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 117857048, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 89810746 | HCID 89810746 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Sodium Thiosulfate | HCID 24477 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 117857048 | HCID 117857048 | 94% |
Reaction Steps
A solution of 3-(2,2,2-trifluoroethyl)thieno[2,3-d]pyrimidin-4(3H)-one (2 g, 8.54 mmol) and bromine (0.484 ml, 9.39 mmol) in DMF (20 ml) at 0° C. was stirred for 60 min. The reaction mixture was diluted with 1:1 sodium thiosulfate (25% aqueous solution)/saturated sodium bicarbonate (aq) solution (100 ml) and extracted with ethyl acetate (100 ml). The concentrated crude product was purified by flash chromatography (0-60% ethyl acetate/cyclohexane) to give the title compound (2.5 g, 94%). LCMS RT=1.16 min, M+H+=312.9/314.9.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156853B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-7b597e1820a34b4c8dec3c45eb0312b0 |
| Source note | uspto-grants-2015_10 |