HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 131722755, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,4-Dichloro-2-butyne | HCID 13182 | — |
| Reactant | HCID 9926519 | HCID 9926519 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131722755 | HCID 131722755 | — |
Reaction Steps
Potassium carbonate (311 mg, 2.2 mmol) and 1,4 dichloro-2-butyne (275 mg, 2.2 mol) in DMF (3 ml) were heated to 50° C. prior to the dropwise addition of the product from Example 185, Step a (200 mg, 0.75 mmol) in DMF (2 ml). The reaction mixture was left to stir for 2 hours. Cooled and partitioned (ethyl acetate/water). The organic layer was washed (H2O, brine), dried MgSO4) and evaporated in vacuo. Purified via silica gel chromatography using 50/50 ethyl acetate/hexane to elute. 1H NMR (250 MHz, CDCl3) δ1.93 (1 H, m), 2.11-2.16 (3 H, m), 2.42 (2 H, m), 4.2 (2 H, m), 5.10 (2 H, m), 7.50-7.59 (3 H, m), 7.84 (1 H, s), 8.47 (2 H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06255305B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-0d4003ad95f9474e898341baad35912b |
| Source note | uspto-grants-2001_07 |