HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 63803879, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Fluorobenzaldehyde | HCID 68023 | — |
| Reactant | HCID 178506226 | HCID 178506226 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 63803879 | HCID 63803879 | 87% |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
A mixture of 5-trifluoromethyl-pyridine-2-thiol (6.99 g, 39.0 mmol), 4-fluorobenzaldehyde (4.79 g, 38.6 mmol), anhydrous K2CO3 (8.16 g, 59.1 mmol) and DMF (70 mL) was heated at 110° C. for 18 h. The mixture was cooled to room temperature and partitioned between MTBE and water. The phases were separated. The organic extracts were combined, dried over Na2SO4, filtered and evaporated to give a crude product which was purified by flash column chromatography (eluent: 5% MTBE in petroleum ether). Evaporation of the appropriate fractions gave the product (9.47 g, 87% yield). 1H NMR (CDCl3) δ 10.06 (s, 1H), 8.69-8.66 (m, 1H), 7.97-7.92 (m, 2H), 7.78-7.72 (m, 3H), 7.23-7.16 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07329656B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-aade7da85b054679afdbb4e4882f4c5f |
| Source note | uspto-grants-2008_02 |