HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 71513875, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | p-Chlorophenoxyacetyl chloride | HCID 77771 | — |
| Reactant | HCID 117642421 | HCID 117642421 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 71513875 | HCID 71513875 | 80.2% |
Reaction Steps
To a suspension of Example 15 (0.2 mmol) and potassium carbonate (0.2 mmol) in 1,4-dioxane (5 mL) was added 4-chlorophenoxyacetyl chloride (0.2 mmol). The reaction mixture was stirred at room temperature for 1 hour. After concentration under reduced pressure, the crude residue was purified by flash chromatography on silica, the mobile phase being a mixture of methanol and dichloromethane (in a ratio of 1:60), yielding the pure title compound (80 mg, 80%) as a yellowish solid. MS (m/z) 499.2 [M+H]+ (100%). 1H NMR δH (300 MHz, DMSO-d6, 25° C.) 7.72 (dd, J 8.4, 5.6 Hz, 2H), 7.38 (t, J 8.7 Hz, 2H), 7.30 (d, J 8.8 Hz, 2H), 7.08 (s, 2H, NH2), 6.89 (d, J 8.8 Hz, 2H), 4.76 (s, 2H), 3.34 (br s, 4H), 3.20 (br s, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227984B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-0ab51a657f5b49ab8ab9c4cc36aaec92 |
| Source note | uspto-grants-2016_01 |