HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Phosphate, Tribasic → HCID 66807421, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | 3-Bromo-4-(trifluoromethyl)pyridine | HCID 19937263 | — |
| Reactant | 8-fluoro-3,4-dihydro-2H-benzo[4,5]thieno[3,2-c]pyridin-1-one | HCID 89964175 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66807421 | HCID 66807421 | 9.1% |
Reaction Steps
Using analogous conditions and workup as described for the preparation of Example 1A above, 8-fluoro-3,4-dihydro-2H-benzo[4,5]thieno[3,2-c]pyridin-1-one (I-50g: 100 mg, 0.452 mmol) was reacted with 3-bromo-4-trifluoromethylpyridine (102.26 mg, 0.452 mmol), 1,4-dioxane (3 mL), copper iodide (8.58 mg, 0.0452 mmol), trans-N,N′-dimethyl-cyclohexyl-1,2-diamine (19.25 mg, 0.135 mmol) and potassium phosphate (286.56 mg, 1.35 mmol) in a vial at 115° C. overnight under nitrogen atmosphere to afford the crude product. Purification by preparative HPLC afforded 15 mg of the product (9.09% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946260B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-dcd7f1f103704fb89cdb17972ce49c94 |
| Source note | uspto-grants-2015_02 |